CN111905836A - Porous plastic chemical reagent carrier and preparation method and application thereof - Google Patents

Porous plastic chemical reagent carrier and preparation method and application thereof Download PDF

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Publication number
CN111905836A
CN111905836A CN202010819698.5A CN202010819698A CN111905836A CN 111905836 A CN111905836 A CN 111905836A CN 202010819698 A CN202010819698 A CN 202010819698A CN 111905836 A CN111905836 A CN 111905836A
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reagent
porous
carrier
porous plastic
chemical reagent
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胥波
齐义舟
李婷婷
齐培州
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Shanghai Group Wave Intelligent Instrument Technology Co Ltd
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Shanghai Group Wave Intelligent Instrument Technology Co Ltd
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Abstract

The invention provides a porous plastic chemical reagent carrier and a preparation method and application thereof. The chemical reagent carrier prepared by the technical scheme changes the use form of the chemical reagent, so that solid, semisolid and viscous liquid which are difficult to operate and accurately weigh can be conveniently measured, the preparation process is simple and convenient, and a solvent which is not friendly to the environment is not introduced in the preparation process, so that the preparation method is easy for industrial production and has better environment-friendly effect.

Description

Porous plastic chemical reagent carrier and preparation method and application thereof
Technical Field
The invention relates to the technical field of chemical reagent loading, in particular to a porous plastic chemical reagent carrier and a preparation method and application thereof.
Background
The chemical synthesis is more and more widely applied to various fields such as medicine, pesticide, fine chemical engineering, materials, sensors, aerospace and the like. Despite significant advances, chemical synthesis is still currently a rather dangerous, labor intensive industry. In particular, the safety hazards inherent in the handling of hazardous chemicals make the chemist in the field of automation of chemical synthesis a prejudice. While automation has revolutionized many industrial and laboratory tasks, in practical applications, full automation of chemical synthesis remains highly challenging, and in most schools and industrial laboratories, the vast majority of chemical experiments are still done manually. Many conventional chemical processing tasks are still difficult for automated machines, downloading or designing synthetic protocols, and can be performed fully automatically in a local synthesizer, which is the dream of synthetic chemists.
Because the variety of chemicals involved in chemical synthesis is various, and it is very time-consuming and labor-consuming to weigh a small amount or a trace amount of chemical reagents, automatic synthesis is realized, and firstly, thousands of reagents need to be standardized, especially, the dosage of the reagents is standardized, which is beneficial to a robot system controlled by an algorithm. Automated removal of low viscosity liquids is relatively easy, however, solid, semi-solid, and viscous liquid reagents face significant challenges. In recent years, automated synthesis has been greatly advanced, but related research at home and abroad has no relatively general method for processing thousands of chemicals with different forms, so that highly automated synthesis cannot be realized.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides an ultrahigh molecular weight porous plastic chemical reagent carrier and a preparation method and application thereof, and the following technical scheme is specifically adopted:
the invention provides in a first aspect a porous plastic chemical reagent carrier in the form of a porous solid block structure;
further, the porous plastic chemical reagent carrier is of a tablet-like cylindrical structure, a spherical structure or a cubic structure; more preferably, the tablet-like cylindrical structure porous plastic chemical reagent carrier has a pore volume of 0.3-0.6 ml/g and a total pore area of 20-25 m2(iv)/g, having an average pore diameter of 70 to 80nm, a bulk density of 0.5 to 1.0g/ml at 0.5 to 1psi, and a porosity of 20 to 30%; preferably, itThe pore volume is 0.4298 ml/g; the total pore area is 23.780m2(ii)/g; the average pore diameter is 72.3 nm; the bulk density of the composite material is 0.6069g/ml under 0.5-1 psi; its porosity is 26.0850%;
further, the specifications of the tablet-like cylindrical structure porous plastic chemical reagent carrier are as follows: the inner diameter is 5.1-9 mm and the height is 2.5-4 mm; furthermore, the weight of the porous plastic chemical reagent carrier with the tablet-like cylindrical structure is 30 mg/tablet or 150 mg/tablet;
further, the porous plastic is a material with high wear resistance and high chemical inertness, including but not limited to ultra-high molecular weight porous polyethylene, ultra-high molecular weight porous polypropylene, ultra-high molecular weight polytetrafluoroethylene or ultra-high molecular weight polyvinylidene fluoride;
further, the chemical reagent is a solid reagent or a liquid reagent; further, the solid reagent is a soluble solid or an insoluble solid; still further, the liquid reagents include, but are not limited to, viscous liquids;
the second aspect of the invention provides a preparation method of the porous plastic chemical reagent carrier, which comprises the following steps: adding the plastic powder into a cylindrical stainless steel grinding tool, heating to 140-155 ℃ under normal pressure, rapidly cooling to room temperature, and demolding to obtain the plastic powder;
further, the diameter of the porous plastic powder is 10-100 micrometers, and the molecular weight of the porous plastic powder is more than 100 ten thousand;
further, the inner diameter of the cylindrical stainless steel grinding tool is 5.1-9 mm, and the height of the cylindrical stainless steel grinding tool is 2.5-4 mm; specifically, the size of the cylindrical stainless steel grinding tool: an inner diameter of 5.1mm and a height of 2.5mm, an inner diameter of 7.4mm and a height of 2.5mm, or an inner diameter of 9mm and a height of 4 mm;
in a third aspect the invention provides the use of a porous plastic chemical reagent carrier, characterised in that it is used to carry a chemical reagent;
further, the chemical reagent is a solid reagent or a liquid reagent; further, the solid reagent is a soluble solid reagent or an insoluble solid reagent; still further, the liquid reagent includes, but is not limited to, a non-viscous liquid reagent or a viscous liquid reagent.
The fourth aspect of the invention provides a porous plastic chemical reagent, comprising the above porous plastic chemical reagent carrier and chemical reagent carried by the same, further, the amount of substance of the chemical reagent carried by the porous plastic chemical reagent carrier is determined;
further, the amount of the chemical reagent substance loaded on the porous plastic chemical reagent carrier is 0.001-10.0 mol; furthermore, the amount of the chemical reagent substance loaded on the porous plastic chemical reagent carrier is 0.01 mu mol-1.0 mol; further, the amount of the substance of the chemical agent supported by the porous plastic chemical agent carrier is 0.001. mu. mol, 0.002. mu. mol, 0.005. mu. mol, 0.01. mu. mol, 0.02. mu. mol, 0.05. mu. mol, 0.1. mu. mol, 0.2. mu. mol, 0.5. mu. mol, 1. mu. mol, 2. mu. mol, 5. mu. mol, 10. mu. mol, 20. mu. mol, 50. mu. mol, 100. mu. mol, 200. mu. mol, 500. mu. mol, 1mmol, 2mmol, 5mmol, 10mmol, 20mmol, 50mmol, 100mmol, 200mmol, 500mmol, or 1 mol;
further, the porous plastic chemical reagent is a porous soluble solid reagent, a porous insoluble solid reagent or a porous liquid reagent; still further, the porous liquid reagent includes, but is not limited to, a porous non-viscous liquid reagent or a porous viscous liquid reagent;
further, the preparation method of the porous soluble solid reagent comprises the following steps:
s1: dissolving soluble solid in a low-boiling-point good solvent with the mass of 0.1-100% to prepare a solution; preferably, the good solvent includes, but is not limited to, ethanol, chloroform or water;
s2: using a liquid transfer device to transfer the solution obtained in the step S1 to be dropped on the porous plastic chemical reagent carrier, and obtaining a porous carrier of the loading solution after the solution is completely adsorbed on the carrier; preferably, the pipetting device is a pipette gun;
s3: drying the porous carrier of the loading solution obtained in the step S2 in vacuum under the pressure of 1mmHg and the temperature of 0-60 ℃ until the solvent is completely volatilized to obtain a porous soluble solid reagent;
further, in the porous soluble solid reagent, the amount of the substance of the soluble solid reagent loaded on the porous plastic chemical reagent carrier is 0.001 mu mol-10.0 mol; further, the amount of the soluble solid reagent substance loaded on the porous plastic chemical reagent carrier is 0.01 mu mol-1.0 mol; further, the amount of the soluble solid reagent substance supported by the porous plastic chemical reagent carrier is 0.001. mu. mol, 0.002. mu. mol, 0.005. mu. mol, 0.01. mu. mol, 0.02. mu. mol, 0.05. mu. mol, 0.1. mu. mol, 0.2. mu. mol, 0.5. mu. mol, 1. mu. mol, 2. mu. mol, 5. mu. mol, 10. mu. mol, 20. mu. mol, 50. mu. mol, 100. mu. mol, 200. mu. mol, 500. mu. mol, 1mmol, 2mmol, 5mmol, 10mmol, 20mmol, 50mmol, 100mmol, 200mmol, 500mmol, or 1 mol;
further, the preparation method of the porous insoluble solid reagent comprises the following steps:
s1: grinding the insoluble solid agent to a powder of less than 5 microns;
s2: suspending the powder in an organic solvent with the mass 8-50 times of that of the powder to obtain a suspension, adding the suspension into the porous plastic chemical reagent carrier at the temperature of 0-30 ℃ at the speed of 300-600 r/min while stirring, and fully stirring for 1-24 hours to enable the powder to be fully adsorbed to the carrier; preferably, the organic solvent includes, but is not limited to, ethanol, petroleum ether, toluene, tetrahydrofuran, or dichloromethane;
s3: continuously stirring the carrier loaded with the insoluble solid reagent obtained in the step S2 in a clean and same organic solvent at the same speed and temperature for 10-24 hours to wash away powder which is not adsorbed on the surface of the carrier, so as to obtain a porous insoluble solid reagent; further, in the porous insoluble solid reagent, the amount of the insoluble solid reagent substance loaded on the porous plastic chemical reagent carrier is 0.001 mu mol-10.0 mol; further, the amount of the insoluble solid reagent substance carried by the porous plastic chemical reagent carrier is 0.01 mu mol to 1.0 mol; further, the amount of the insoluble solid reagent substance supported by the porous plastic chemical reagent carrier is 0.001. mu. mol, 0.002. mu. mol, 0.005. mu. mol, 0.01. mu. mol, 0.02. mu. mol, 0.05. mu. mol, 0.1. mu. mol, 0.2. mu. mol, 0.5. mu. mol, 1. mu. mol, 2. mu. mol, 5. mu. mol, 10. mu. mol, 20. mu. mol, 50. mu. mol, 100. mu. mol, 200. mu. mol, 500. mu. mol, 1mmol, 2mmol, 5mmol, 10mmol, 20mmol, 50mmol, 100mmol, 200mmol, 500mmol, or 1 mol.
Further, the loading method of the porous liquid reagent comprises the following steps:
s1: directly sucking a liquid reagent by using a liquid transfer device or sucking a liquid diluted to 5-100 times of the mass of the liquid reagent in a low-boiling-point good solvent, and dripping the liquid reagent on the porous plastic chemical reagent carrier to obtain a liquid reagent-loaded porous carrier after the carrier fully adsorbs the liquid reagent; preferably, the pipetting device is a pipette gun;
s2: vacuum drying the porous carrier of the loading solution obtained in the step S2 for 10-60 min at the pressure of 1mmHg and the temperature of 0-60 ℃ to obtain a porous liquid reagent; further, in the porous liquid reagent, the amount of the insoluble solid reagent substance loaded by the porous plastic chemical reagent carrier is 0.001 mu mol-10.0 mol; further, the amount of the insoluble solid reagent substance carried by the porous plastic chemical reagent carrier is 0.01 mu mol to 1.0 mol; further, the amount of said defined liquid reagent substance is 0.01. mu. mol, 0.02. mu. mol, 0.05. mu. mol, 0.1. mu. mol, 0.2. mu. mol, 0.5. mu. mol, 1. mu. mol, 2. mu. mol, 5. mu. mol, 10. mu. mol, 20. mu. mol, 50. mu. mol, 100. mu. mol, 200. mu. mol, 500. mu. mol, 1mmol, 2mmol, 5mmol, 10mmol, 20mmol, 50mmol, 100mmol, 200mmol, 500mmol or 1 mol.
Advantageous effects
The technical scheme adopted by the invention has the following technical effects:
the strength and the loading capacity of the chemical reagent carrier are improved: porous plastics, in particular ultra High molecular weight Polyethylene (HDPE) are white powder or granular products. No toxicity and no smell, the crystallinity is 80-90%, the softening point is 125-l 35 ℃, and the use temperature can reach 110 ℃; the hardness, tensile strength and creep property are all superior to those of low-density polyethylene; the wear resistance, the electrical insulation, the toughness and the cold resistance are good; good chemical stability, no solubility in any organic solvent at room temperature, and low corrosion resistance to acid, alkali and various salts. Therefore, the carrier used for preparing the porous polymer chemical reagent has the following excellent technical effects:
the use form of the chemical reagent is changed, for example, the liquid or soluble solid reagent is changed into the solid reagent, the reagent which is difficult to treat such as viscous liquid is changed into the solid reagent, the use is convenient, the quantification is convenient, and the reagent is easy to separate from other chemical reagents; the transportation is convenient, and the contact between scientific research personnel and toxic reagents can be reduced; the mechanical strength of the chemical reagent is obviously improved; the load capacity of unit mass is large, the chemical reaction is facilitated, and the method can be widely applied to various chemical reactions.
The preparation method of the porous plastic carrier is simpler and more convenient: the porous plastic carrier can be obtained by operations of heating, sintering, cooling and the like under normal pressure; the method for loading the chemical reagent is simple and convenient: chemical reagents can be loaded by dripping, absorbing or stirring at normal temperature and normal pressure; and a solvent which is not friendly to the environment is not introduced in the preparation process, so that the environment-friendly effect is better.
Drawings
FIG. 1 is a photograph of a blank chemical reagent carrier taken from a real object and a scanning SEM image
FIG. 2 morphology of Pd/C @ tab prepared in example 2
FIG. 3 kinetic graph comparison of reagent tablets and reagent powders
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
EXAMPLE 1 preparation of ultra high molecular weight porous polyethylene chemical agent Carrier
The method comprises the following steps: adding ultra-high molecular weight polyethylene powder with diameter of 50 μm and molecular weight of more than 100 ten thousand into cylindrical stainless steel grinding tool with inner diameter of 5.1, 7.4 or 9mm and height of 2.5mm or 4mm, heating to 150 deg.C under normal pressure, rapidly cooling to room temperature, and demolding. The prepared ultrahigh molecular weight porous polyethylene chemical reagent carrier has high hardness, hardly cracks in the stirring process, but can be cut by a sharp knife to prepare various shapes, and the picture of the catalyst carrier with two diameters prepared in the embodiment 1 of the invention is shown in figure 1 a; the obtained carrier was placed under a scanning electron microscope, and an SEM image obtained is shown in FIG. 1 b.
EXAMPLE 2 quantitative preparation of porous polyethylene chemical reagent sheet
(1)Pd(OAc)2Preparation of a reagent tablet: weighing 6.74mg Pd (OAc)2Dissolving in 600 μ L chloroform, mixing well to obtain Pd (OAc)2Solution, using a pipette to precisely suck 20 μ L of the above solution, respectively, dropping the solution on 30 blank loading pieces (size: 5.1mm in diameter and 2.5mm in height, 30 mg/piece), fully absorbing, and vacuum drying to obtain reagent piece containing Pd (OAc)2The content of (B) is 1. mu. mol/tablet.
(2) Preparation of XPhos reagent sheet: 14.28mg of XPhos is weighed, dissolved in 600 mu L of chloroform and uniformly mixed to prepare XPhos solution, 20 mu L of the solution is respectively and precisely absorbed by a pipette and respectively dripped on 30 blank loading sheets (the size: the diameter is 5.1mm and the height is 2.5mm, and the concentration is 30 mg/sheet), and after the solution is fully absorbed, the XPhos content in the prepared reagent sheet is 1 mu mol/sheet after vacuum drying.
(3)K3PO4Preparation of a reagent tablet: weighing 636.80mg K3PO4Dissolving in 1.8mL water, mixing, dripping 60 μ L solution onto 30 blank loading pieces (size: 9.0mm 4mm, 150 mg/piece) with pipette gun, dripping 20 μ L ethanol to make the water solution absorbed by the loading pieces, and vacuum drying to obtain reagent piece K3PO4The content of (B) was 0.1 mmol/tablet.
(4) Preparation of various ligand reagent tablets. The preparation method is the same as K3PO4And (4) preparing. Respectively adding PPh3SPhos, XtantPhos, DPEPhos, and Dppf were prepared as chloroform solutions and prepared into reagent tablets (size: 5.1mm in diameter by 2.5mm in height, 30 mg/tablet) each having a ligand content of 1. mu. mol/tablet.
(5) Preparation of sodium tert-butoxide reagent tablets: the preparation method is the same as K3PO4And (4) preparing. Weighing sodium tert-butoxide to prepare a THF solution, and preparing 0.05 mmol/tablet (size: 5.1mm in diameter and 2.5mm in height, 30 mg/tablet) and 0.2 mmol/tablet (size: 5.1mm in diameter and 2.5mm in height, 30 mg/tablet) of the two standard reagent tablets respectively. The preparation method is the same as K3PO4And (4) preparing.
(6) Preparation of Pd/C reagent tablets: grinding 600.0mg of micro Pd/C powder (which is commercially available and has a Pd content of 10 wt/wt%) into powder with a particle size of less than or equal to 5 microns, suspending the powder in 150ml of ethanol, and adding 100 pieces (with the size: 5.1mm in diameter and 2.5mm in height and 30 mg/piece) of porous plastic chemical reagent carriers while stirring, wherein the stirring speed is 500r/min, the stirring temperature is room temperature, and the stirring time is 24 hours; fully stirring to fully load the reagent to the carrier until the suspension becomes clear, then taking out the loaded reagent, and continuously stirring for 12 hours in clean 100mL ethanol at the same speed and temperature to wash off the redundant reagent on the surface of the catalyst carrier, thus obtaining Pd/C @ tab, wherein the maximum load of the carrier to micron Pd/C is 2 mu mol/piece; preparation the quantitative Pd/C @ tab photo is shown in FIG. 2.
Example 3 Suzuki reaction and kinetics study thereof
A reaction tube was charged with the powdered reagent substrate 4-bromoanisole (0.1mmol,18.7mg), 1-naphthalene boronic acid (0.1mmol,17.2mg), and the palladium acetate reagent tablet (1 tablet), XPhos reagent tablet (2 tablets), K prepared in example 23PO4Reagent tablets (2 tablets), 1.5mL of ethanol aqueous solution (the volume ratio of ethanol to water is 9: 1); the other reaction tube was charged with the powdered reagents 4-bromoanisole (0.1mmol,18.7mg), 1-naphthaleneboronic acid (0.1mmol,17.2mg), palladium acetate (1. mu. mol, 0.22mg), XPhos (2. mu. mol, 0.95mg), K3PO4(0.2mmol, 42.45mg), and 1.5mL of an aqueous ethanol solution (ethanol: water volume ratio of 9: 1). Stirring the two reaction tubes at 60 deg.C, detecting reaction conversion rate by GC-MS when the reaction is carried out for 15min, 30min, 1h, 2h and 4h respectively, to obtain reaction kinetic diagram (shown in FIG. 3), and it can be seen from FIG. 3 that palladium acetate reagent sheet, XPhos reagent sheet and K are used3PO4Reagent sheet and palladium acetate, XPhos and K3PO4The powders were reacted separately, with very similar conversion rates at the same time, demonstrating that the introduction of the reagent tablets did not affect the release of the reagent and the rate of reaction.
Example 4 Supported sheets for other chemical Agents
Using a very similar method, reagent tablets as shown in table 1 were prepared:
Figure BDA0002634010870000091
example 5: olefin metathesis
To the reaction flask was added a solution of 1-octene in dichloromethane (abbreviated DCM) (2mL, 0.1mol/L), ethyl acrylate (173.9. mu.L, 1.6mmol) and 2 Grubbs catalyst support pieces (0.001 mmol/piece). The mixture was stirred at room temperature under argon for 5 hours. After removal of the tablets, the reaction mixture was evaporated on a high vacuum pump and the crude product was purified by flash chromatography on silica gel column (eluent: hexane/ethyl acetate v/v ═ 20:1) to give the compound 2-en-onyl ethyl ester (35.4mg, 96% yield). Identified by nuclear magnetic spectrum, the compound 2-alkene nonyl ethyl ester1H-NMR(400MHz,CDCl3)：7.04-6.91(m,1H),5.81(d,J＝15.7Hz,1H),4.19(q,J＝6.8Hz,2H),2.19(d,J＝6.5Hz,2H),1.50-1.20(m,11H),0.89(t,J＝6.8Hz,3H)。
Example 6: mitsunobu reaction
To the reaction flask was added a solution of p-nitrobenzoic acid in THF, phenethyl alcohol (24.0 μ L, 0.2mmol), 2 PPh tablets3-loading pellet (0.2 mmol/pellet) and 2 diethyl azodicarboxylate loading pellets (DEAD-loading pellet, 0.2 mmol/pellet); the mixture was stirred at room temperature overnight, after removal of the tablets, the reaction mixture was evaporated on a high vacuum pump and the crude product was purified by flash chromatography on silica gel column (eluent: hexane/ethyl acetate v/v ═ 10:1) to give the compound, phenethyl-nitrobenzoate (44.1mg, 81% yield). By nuclear magnetic spectrum identification, the compound is p-nitro benzoic acid phenethyl ester1H NMR(400MHz,CDCl3)：8.28(d,J＝8.7Hz,2H),8.17(d,J＝8.7Hz,2H),7.40-7.19(m,5H),4.59(t,J＝6.9Hz,2H),3.11(t,J＝6.9Hz,2H)。
Example 7: trifluoromethylation reaction
To the reaction flask was added methyl benzoate (25.0. mu.L, 0.2mmol), trifluoromethyl trimethylsilane (abbreviated as TMS-CF)332.5 μ L, 0.23mmol) and 1 cesium fluoride support (CsF-support, 0.002 mmol/plate), the mixture was stirred at room temperature and passed through19F NMR monitoring; after completion, the resulting product was extracted with ether (10mL), and ether was removed to give the product, trifluoroacetophenone (44.1mg, 81% yield), which was subjected to nuclear magnetic spectrum identification,1H NMR(400MHz,CDCl3)8.08(d,J＝8.4Hz,2H),7.72(t,J＝6.9Hz,1H),7.56(t,J＝7.9Hz,2H)；19F NMR(400MHz,CDCl3)71.42(s)。
example 8: cyclization reaction
To the reaction flask were added ethanol-free chloroform (0.5mol/L, 1mL), styrene (23.0. mu.L, 0.2mmol), and nitromethylbenzene, 1 tablet of 1, 4-diazabicyclo [2.2.2 ]]Octane (DABCO-supported, 0.1 mmol/plate), and the mixture was stirred at 60 ℃ for 40 hours. The solvent was then removed, the residue dissolved in ether (10mL) and washed with water (3X 10mL), NaOH (1M, 3X 10mL) and brine (3X 10mL), and the organic layer was Na-filtered2SO3Drying and concentrating; the crude product was purified by silica gel column chromatography (eluent: hexane/ethyl acetate v/v ═ 10:1) to give the product 3, 5-diphenyl-4, 5-dihydroisoxazolopterin (35.7mg, 80% yield). The product is identified by a nuclear magnetic spectrum,1H NMR(400MHz,CDCl3)7.73-7.66(m,2H),7.45-7.29(m,8H),5.74(dd,J＝11.0,8.2Hz,1H),3.78(dd,J＝16.6,11.0Hz,1H),3.35(dd,J＝16.6,8.2Hz,1H).
example 9: substitution reaction
To the reaction flask was added a solution of 1 '-bromo-2', 3', 6', 2, 3, 4, 6-heptyl-o-acetyl- α -d-lactose in acetonitrile (0.1mol/L, 2mL), ethylene glycol (278.8 μ L, 5mmol) and 4 pieces of silver p-toluenesulfonate (AgOTs-supported sheets, 0.1 mmol/piece), the mixture was stirred at room temperature for 3 hours, after filtering the solid, the solvent was evaporated, and the crude product was dissolved in ethyl acetate (ethyl acetate)Ester, 5mL), the solution was washed with water (3 × 5mL), and the aqueous layer was back-extracted with ethyl acetate (10mL), the combined organic layers were dried over anhydrous sodium sulfate and concentrated, and the crude product was purified by silica gel column chromatography (eluent: hexane/ethyl acetate v/v ═ 1: 1) to obtain the product disaccharide shown in formula 24 (86.5mg, 65% yield). The product is identified by nuclear magnetic spectrum,1H NMR(400MHz,CDCl3)5.35(d,J＝3.4Hz,1H),5.21(t,J＝9.3Hz,1H),5.12(dd,J＝10.4,7.8Hz,1H),5.00-4.87(m,2H),4.58-4.45(m,3H),4.09(ddd,J＝23.6,11.7,5.2Hz,4H),3.92-3.82(m,2H),3.82-3.63(m,5H),2.16(s,3H),2.13(s,3H),2.08-2.03(m,12H),1.97(s,3H)。
example 10: hydrogenation reaction
To a reaction flask, a solution of N-benzyloxycarbonyl-L-phenylalanine (N-Cbz-L-phenylalanine) in ethanol (0.1mol/L, 2mL) was added 6 Pd/C-loaded sheets (0.001 mmol/tablet). The mixture was stirred under an atmosphere of H2 (balloon) at room temperature for 4 hours. After removal of the tablets, the combined solutions were concentrated in vacuo to give the pure product, which was phenylalanine (29.5mg, 89%) without further purification. The product is identified by a nuclear magnetic spectrum,1H NMR(400MHz,D2O)7.44-7.26(m,5H),3.96(dd,J＝8.0,5.2Hz,1H),3.26(dd,J＝14.5,5.2Hz,1H),3.10(dd,J＝14.5,8.0Hz,1H)。
EXAMPLE 5 reductive amination
To the reaction flask, tetrahydro-4H-pyran-4-one (18.5. mu.L, 0.2mmol), benzylamine (24.0. mu.L, 0.22mmol) and titanium isopropoxide (94.7. mu.L, 0.32mmol) were added and stirred. At room temperature for 3 hours. Thereafter, 3 NaBH tablets were added4Load sheet (0.1 mmol/sheet). The mixture was stirred for 24 hours. After removal of the tablets, sodium hydroxide solution was added and the mixture was extracted with DCM (3X 5mL) and then washed with brine (5 mL). The combined organic layers were dried over anhydrous sodium sulfate and concentrated. The crude product was purified by silica gel column chromatography (eluent: hexane/ethyl acetate v/v ═ 5:1) to give N-benzyl-tetrahydropyran-4-amine (35.8mg, yield 93%). The product is identified by a nuclear magnetic spectrum,1H NMR(CDCl3)7.22-7.36(m,5H),3.98(d,J＝11.7Hz,2H),3.83(s,2H),3.38(t,J＝11.6Hz,2H),2.67-2.77(m,1H)),1.86(d,J＝11.5Hz,2H),1.38-1.50(m,2H)。
EXAMPLE 5 condensation reaction
To the reaction flask was added propiolic acid (13.5. mu.L, 0.22mmol), N-methylaniline (21.7. mu.L, 0.2mmol), 1 dicyclohexylcarbodiimide support (DCC-support, 0.15 mmol/plate) and 2 4-dimethylaminopyridine (DMAP-support, 0.01 mmol/plate) and DCM (2 mL). The mixture was stirred at room temperature overnight. After filtration of the solid, the reaction mixture was evaporated on a high vacuum pump and the crude product was purified by flash chromatography on silica gel column (eluent: hexane/ethyl acetate v/v ═ 10:1) to give the product N-phenyl-N-methyl-propiolic acid amine (27.8mg, 87% yield). The product is identified by a nuclear magnetic spectrum,1H NMR(400MHz,CDCl3)7.45-7.36(m,3H),7.29(dd,J＝7.7,1.5Hz,2H),3.34(s,3H),2.81(s,1H)。
EXAMPLE 5 reduction reaction
To the reaction flask were added an ethanol solution of estrone (0.1mol/L, 2mL) and 2 tablets of NaBH4Load sheet (0.1 mmol/tablet). The mixture was stirred at room temperature for 2 h. After removal of the tablets, water (10mL) was added and the aqueous phase was extracted with ethyl acetate (3X 5 mL). The combined organic layers were dried over anhydrous sodium sulfate and concentrated. The crude product was purified by silica gel column chromatography (eluent: hexane/ethyl acetate v/v ═ 2:1) to give sterol (49.5mg, 91% yield). The product is identified by a nuclear magnetic spectrum,1H NMR(400MHz,Methanol-d4)7.07(d,J＝8.4Hz,1H),6.56-6.43(m,2H),3.65(t,J＝8.6Hz,1H),2.76(d,J＝5.0Hz,2H),2.29(d,J＝15.8Hz,1H),2.07-1.81(m,3H),1.69(dd,J＝7.0,2.6Hz,1H),1.57-1.13(m,8H),0.77(s,3H)。
EXAMPLE 5 allylation reaction
To the reaction flask was added 4-methoxyphenol 36 in DMF (0.1mol/L, 2mL), allyl bromide (20.8. mu.L, 0.24mmol) and 2 sheets of K2CO3Loading sheet (0.2 mmol/sheet) the mixture was stirred at 70 ℃ for 16 h. After removal of the tablets, the reaction was quenched with water (5mL) and extracted with ether (2X 5 mL). The combined organic extracts were washed with brine (2 × 5mL), dried over anhydrous sodium sulfate and concentrated. The crude product was purified by silica gel column chromatographyAlkylation (eluent: hexane/ethyl acetate v/v ═ 10:1) gave p-methoxyphenol allyl ether (32.1mg, 98% yield). The product is identified by a nuclear magnetic spectrum,1H NMR(400MHz,CDCl3)6.88-6.79(m,4H),6.05(tdd,J＝17.3,10.6,5.3Hz,1H),5.40(ddd,J＝17.3,3.0Hz,1.3Hz,1H),5.27(ddd,J＝10.6,3.0Hz,1.3Hz,1H),4.48(td,J＝1.3and 5.3Hz,2H),3.76(s,3H)。
EXAMPLE 5 condensation reaction
Injecting bicyclo [2.2.1 ] into a reaction flask]Hept-5-ene-2-carbaldehyde (23.7. mu.L, 0.2mol), malononitrile (12.6. mu.L, 0.2mmol), 1 pyridine-loaded slide (Py-slide, 0.04 mmol/slide), glacial acetic acid (2 mL). The mixture was stirred at room temperature overnight. After removal of the tablets, the reaction was quenched with water (5mL) and extracted with ethyl acetate (3X 5 mL). The combined organic extracts were washed with water (10mL), dried over anhydrous sodium sulfate and concentrated. The crude product was purified by silica gel column chromatography (eluent: hexane/ethyl acetate v/v ═ 10:1) to give the product bicyclo [2.2.1]-5-hepten-2-methylenepropanedicyano (32.5mg, 88%). The product is identified by a nuclear magnetic spectrum,1H NMR(400MHz,400MHz,CDCl3)6.85(d,J＝11.0Hz,1H),6.36(dd,J＝5.7,3.1Hz,1H),6.00(dd,J＝5.7,2.8Hz,1H),3.37-3.28(m,1H),3.07(d,J＝15.7Hz,2H),2.19(ddd,J＝12.4,9.1,3.5Hz,1H),1.60(d,J＝8.1Hz,1H),1.42(d,J＝8.7Hz,1H),0.96(ddd,J＝12.2,3.8,2.6Hz,1H)。
although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (12)

1. A porous plastic chemical reagent carrier is characterized in that the porous plastic chemical reagent carrier is a porous solid block structure.
2. The porous plastic chemical reagent carrier as claimed in claim 1, wherein the porous plastic chemical reagent carrier has a tablet-like cylindrical structure or a spherical structureOr a cubic structure; preferably, the tablet-like cylindrical structure porous plastic chemical reagent carrier has a pore volume of 0.3-0.6 ml/g and a total pore area of 20-25 m2(iv)/g, having an average pore diameter of 70 to 80nm, a bulk density of 0.5 to 1.0g/ml at 0.5 to 1psi, and a porosity of 20 to 30%; further preferably, the specifications of the tablet-like cylindrical structure porous plastic chemical reagent carrier are as follows: the inner diameter is 5.1-9 mm and the height is 2.5-4 mm; more preferably, the weight of the porous plastic chemical reagent carrier with the tablet-like cylindrical structure is 30 mg/tablet or 150 mg/tablet.
3. The porous plastic chemical reagent carrier of claim 1 or 2, wherein the porous plastic is a material with high wear resistance and high chemical inertness; preferably, it includes, but is not limited to, ultra-high molecular weight porous polyethylene, ultra-high molecular weight porous polypropylene, ultra-high molecular weight polytetrafluoroethylene, or ultra-high molecular weight polyvinylidene fluoride.
4. A porous plastic chemical reagent carrier according to claim 1 or 2, wherein the chemical reagent is a solid reagent or a liquid reagent.
5. A method of making a porous plastic chemical reagent carrier as claimed in any one of claims 1 to 4, comprising the steps of: adding the plastic powder into a cylindrical stainless steel grinding tool, heating to 140-155 ℃ under normal pressure, rapidly cooling to room temperature, and demolding to obtain the plastic powder; preferably, the diameter of the porous plastic powder is 10-100 μm, and the molecular weight of the porous plastic powder is more than 100 ten thousand; preferably, the inner diameter of the cylindrical stainless steel grinding tool is 5.1-9 mm, and the height of the cylindrical stainless steel grinding tool is 2.5-4 mm.
6. Use of a porous plastic chemical reagent carrier according to any of claims 1 to 4 for supporting a chemical reagent.
7. Use of a porous plastic chemical reagent carrier according to claim 6, wherein the chemical reagent is a solid reagent or a liquid reagent.
8. A porous plastic chemical reagent, comprising the porous plastic chemical reagent carrier according to any one of claims 1 to 4 and a chemical reagent carried thereon; preferably, the amount of the substance of the chemical agent carried by the porous plastic chemical agent carrier is determined; further preferably, the amount of the substance of the chemical agent supported by the porous plastic chemical agent carrier is 0.001 μmol to 10.0 mol; more preferably, the amount of the substance of the chemical agent supported by the porous plastic chemical agent carrier is 0.01. mu. mol to 1.0 mol.
9. The porous plastic chemical reagent of claim 8, wherein the porous plastic chemical reagent is a porous dissolvable solid reagent, a porous non-dissolvable solid reagent, or a porous liquid reagent.
10. The porous plastic chemical reagent of claim 9, wherein the preparation method of the porous dissolvable solid reagent comprises the steps of:
s1: dissolving soluble solid in a low-boiling-point good solvent with the mass of 0.1-100% to prepare a solution; preferably, the good solvent includes, but is not limited to, ethanol, chloroform or water;
s2: using a liquid transfer device to transfer the solution obtained in the step S1 to be dropped on the porous plastic chemical reagent carrier, and obtaining a porous carrier of the loading solution after the solution is completely adsorbed on the carrier; preferably, the pipetting device is a pipette gun;
s3: and (3) drying the porous carrier of the loading solution obtained in the step S2 in vacuum under the pressure of 1mmHg and at the temperature of 0-60 ℃, and obtaining the porous soluble solid reagent after the solvent is volatilized.
11. The porous plastic chemical reagent of claim 9, wherein the preparation method of the porous insoluble solid reagent comprises the following steps:
s1: grinding the insoluble solid agent to a powder of less than 5 microns;
s2: suspending the powder in an organic solvent with the mass 8-50 times of that of the powder to obtain a suspension, adding the suspension into the porous plastic chemical reagent carrier at the temperature of 0-30 ℃ at the speed of 300-600 r/min while stirring, and fully stirring for 1-24 hours to enable the powder to be fully adsorbed to the carrier; preferably, the organic solvent includes, but is not limited to, ethanol, petroleum ether, toluene, tetrahydrofuran, or dichloromethane;
s3: and (3) continuously stirring the carrier loaded with the insoluble solid reagent obtained in the step (S2) in a clean and same organic solvent at the same speed and temperature for 10-24 h to wash away the powder which is not adsorbed on the surface of the carrier, so as to obtain the porous insoluble solid reagent.
12. The porous plastic chemical reagent of claim 9, wherein the preparation method of the porous liquid reagent comprises the following steps:
s1: directly sucking a liquid reagent by using a liquid transfer device or sucking a liquid diluted to 5-100 times of the mass of the liquid reagent in a low-boiling-point good solvent, and dripping the liquid reagent on the porous plastic chemical reagent carrier to obtain a liquid reagent-loaded porous carrier after the carrier fully adsorbs the liquid reagent; preferably, the pipetting device is a pipette gun;
s2: and (3) drying the load solution porous carrier obtained in the step S2 in vacuum for 10-60 min at the pressure of 1mmHg and the temperature of 0-60 ℃ to obtain the porous liquid reagent.
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GB1198391A (en) * 1967-05-12 1970-07-15 Bayer Ag Microporous Sheet Structures
US4460530A (en) * 1979-07-09 1984-07-17 Teledyne Industries, Inc. Method for producing porous shaped products
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CA1308356C (en) * 1986-03-31 1992-10-06 Patrick P. Deluca Porous microspheres for drug delivery and method for making same
JPH093236A (en) * 1995-06-15 1997-01-07 Mitsui Petrochem Ind Ltd Porous article of ultrahigh molecular weight polyethylene
JPH0929813A (en) * 1995-07-18 1997-02-04 Mitsubishi Plastics Ind Ltd Manufacture of ultra-high-molecular-weight polyethylene porous material
CN1976751A (en) * 2004-06-28 2007-06-06 H.隆德贝克有限公司 Porous article for delivering chemical substances
CN107649181A (en) * 2017-08-30 2018-02-02 北京工业大学 The preparation and application of a kind of heterogeneous fenton catalyst of support type based on teflon-coated

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1198391A (en) * 1967-05-12 1970-07-15 Bayer Ag Microporous Sheet Structures
US4460530A (en) * 1979-07-09 1984-07-17 Teledyne Industries, Inc. Method for producing porous shaped products
CA1308356C (en) * 1986-03-31 1992-10-06 Patrick P. Deluca Porous microspheres for drug delivery and method for making same
US5118648A (en) * 1988-10-05 1992-06-02 Mobil Oil Corporation Particulate polymer-supported olefin polymerization catalyst
JPH093236A (en) * 1995-06-15 1997-01-07 Mitsui Petrochem Ind Ltd Porous article of ultrahigh molecular weight polyethylene
JPH0929813A (en) * 1995-07-18 1997-02-04 Mitsubishi Plastics Ind Ltd Manufacture of ultra-high-molecular-weight polyethylene porous material
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