CN101851171B - Preparation method of D-panthenol - Google Patents
Preparation method of D-panthenol Download PDFInfo
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- CN101851171B CN101851171B CN2010101635757A CN201010163575A CN101851171B CN 101851171 B CN101851171 B CN 101851171B CN 2010101635757 A CN2010101635757 A CN 2010101635757A CN 201010163575 A CN201010163575 A CN 201010163575A CN 101851171 B CN101851171 B CN 101851171B
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Abstract
The invention relates to a preparation method of D-panthenol. D-(-)-pantolactone is reacted with 3-amino-1-propanol in the absence of solvent to obtain the high-purity D-panthenol, and the overall yield is more than 80%.
Description
Technical field
The present invention relates to a kind of preparation method of D-panthenol, particularly the preparation method of high-optical-purity D-panthenol.
Background technology
Panthenol is commonly called as pro-vitamin B
5, panthenol can be divided into DL body (DL-type), dextrorotatory form (D-type) and 3 kinds of forms of levo form (L-type), wherein has only the dextrorotatory form biologically active, and levo form does not have biological activity.D-panthenol has another name called Dexpanthenol, is a kind of steric isomer with opticity of panthenol, English name dexpanthenol; D-pantothenyl aleohol.
Dexpanthenol (D-panthenol) is the same effect thing of D-pantothenic acid, is the precursor of coenzyme A, is the important vitamines medicine; Get into people's physical efficiency and be converted into pantothenic acid and then synthesize coenzyme A, promote the metabolism of human body protein, fat, carbohydrate, the mucous membrane and the gloss of protection skin surface; Prophylactic generation; D-panthenol is widely used in medicine, food, cosmetic industry as nutritional supplement, concrete preparation such as oral liquid, collyrium, composite vitamin injection, shampoo, mousse, skin cream etc.
The compound method of D-panthenol is modern chemical industry (26) respectively, and 2006, report among the 186-188; Its preparation technology does at ethanol under the condition of solvent for D-(-)-pantoyl lactone and 3-amino-1-propyl alcohol, and after the reacting by heating, concentrating under reduced pressure obtains D-panthenol; This technological reaction needs ethanol as solvent, because D-panthenol is a thick liquid, concentrating under reduced pressure usually can not be removed reaction solvent ethanol fully; Simultaneously product colour be a yellow, and optical value is on the low side, more than all can not the fulfilling medicinal D-panthenol requirement; Especially the injection that contains D-panthenol is higher to specification of quality such as its purity.
Summary of the invention
The purpose of this invention is to provide a kind of simple, economic and technical strong operability, method that productive rate is high prepares the high-optical-purity D-panthenol, total recovery is greater than 80%.
The preparation method of D-panthenol of the present invention; For D-(-)-pantoyl lactone and 3-amino-1-propyl alcohol react under solvent-free condition; Obtain highly purified D-panthenol, described condition of no solvent refers to that reactant has only D-(-)-pantoyl lactone and 3-amino-1-propyl alcohol, does not contain other solvents arbitrarily.
D-(-)-pantoyl lactone can be made with extra care in advance, process for refining be D-(-)-pantoyl lactone through dissolution with solvents, and solvent crystallization purifying behind the activated carbon decolorizing, each step of process for refining can repeat 1～2 time.
In the process for refining of D-(-)-pantoyl lactone, the solvent of dissolving D-(-)-pantoyl lactone can be ETHYLE ACETATE, methylene dichloride, trichloromethane, acetone, methyl acetate etc., ethyl acetate.D-(-)-pantoyl lactone is 1: 1 to 1: 4 with the mass/volume ratio of the solvent of dissolving D-(-)-pantoyl lactone; Be preferably 1: 2.
In the process for refining of D-(-)-pantoyl lactone, the crystallization purification solvent is alkane solvents such as sherwood oil, hexanaphthene, normal heptane, normal hexane, preferred sherwood oil.D-(-)-pantoyl lactone is 1: 1 to 1: 8 with the mass/volume ratio of crystallization purification solvent; Be preferably 1: 4.
In the process for refining of D-(-)-pantoyl lactone; The decoloration active carbon consumption can be 0.01%～0.5% (w/v); The ratio of the weight that decoloration active carbon consumption w/v of the present invention refers to gac and decolouring total liquid volume refers to that as 0.1% the 1g gac joins in the solution that contains D-(-)-pantoyl lactone of 1 liter of volume altogether.
The preparation method of D-panthenol of the present invention, D-(-)-pantoyl lactone and 3-amino-1-propyl alcohol temperature of reaction is 40 ℃～100 ℃, preferred 50 ℃～70 ℃.
The preparation method of D-panthenol of the present invention, as: D-(-)-pantoyl lactone is joined in the reactor drum, add ETHYLE ACETATE, heated and stirred; The back of refluxing adds 0.1% (w/v) activated carbon decolorizing half hour, filters, and adds the sherwood oil crystallization in the filtrating, filters; Again D-(-)-pantoyl lactone is joined in the reactor drum, add ETHYLE ACETATE, heated and stirred; The back of refluxing adds activated carbon decolorizing half hour, filters, and adds the sherwood oil crystallization in the filtrating.Dry.With D-(-)-pantoyl lactone and the 3-amino-1-propyl alcohol reacting by heating 3h after handling, obtain the stickiness liquid of clear and bright colourless easy moisture absorption.
The present invention compared with prior art it is advantageous that: raw material is easy to get, the simple control easily of reaction process; Do not use solvent in the reaction process; Participate in reaction with 3-amino-1-propyl alcohol itself as solvent, reduced cost and environmental pollution, and the fine quality that improves product.
The quality controlling means of D-panthenol of the present invention can for:
These article are D-(2R)-2,4-dihydroxyl-N-(3-hydroxypropyl)-3,3-amide dimethyl butyrate.Calculate with anhydride, contain C
9H
19NO
4Should be 99.0%～101.0%.
[proterties] these article are colourless thick liquid, have draw moist.
These article are very easily dissolving in water, in methyl alcohol and ethanol, is prone to dissolve slightly soluble in ether.
It is an amount of that specific optical rotation is got these article, accurately claims surely, is dissolved in water and quantitatively is diluted to the solution that contains 50mg among every 1ml approximately, measures (two appendix VI of Chinese Pharmacopoeia version in 2005 E) in accordance with the law, and specific optical rotation should be+and 30.0 ° to+32.0 °.
The refractive index of these article of refractive index (two appendix VI of Chinese Pharmacopoeia version in 2005 F) should be 1.495～1.502.
The infrared optical absorption map of these article of [discriminating] (1) should consistent with Dexpanthenol reference substance collection of illustrative plates (two appendix IV of Chinese Pharmacopoeia version in 2005 C).
(2) get the about 0.1g of these article, add water 1ml and make dissolving, add 5 of 1mol/L sodium hydroxide solution 5ml and copper sulfate test solutions, shaken should show mazarine.
(3) get the about 0.1g of these article, add water 10ml and make dissolving, get 1ml, add 1mol/L hydrochloric acid soln 1ml; Heating is 30 minutes in water-bath, and cooling adds the 0.1g oxammonium hydrochloride; Mix, add 1mol/L sodium hydroxide solution 5ml, placed 5 minutes; Behind 1mol/L hydrochloric acid soln adjusting pH to 2.5～3.0, add 1 of iron trichloride test solution, answer displaing amaranth.
[inspection] potential of hydrogen is got these article 0.5g, add water 10ml dissolving after, measure (two appendix VIH of Chinese Pharmacopoeia version in 2005) in accordance with the law, the pH value must not be greater than 10.5.
The clarity of solution and color are got these article 1.0g, add water 20ml dissolving after, solution should be clarified colourless.
Related substance is got these article, be dissolved in water and dilute process contain Dexpanthenol 0.5mg among every 1ml approximately solution as need testing solution; Get need testing solution quantitatively be diluted in right amount contain 2.5 μ g among every 1ml approximately solution as contrast solution.Test according to HPLC (two appendix V of Chinese Pharmacopoeia version in 2005 D).Using octadecylsilane chemically bonded silica to be weighting agent, is moving phase with the 0.1% phosphoric acid solution-acetonitrile (95: 5) of 0.005mol/L sodium pentanesulfonate, and the detection wavelength is 210nm, and number of theoretical plate calculates by the Dexpanthenol peak should be not less than 1500.Get contrast solution 20 μ l and inject liquid chromatograph, regulate detection sensitivity, making the principal constituent peak-to-peak high is 20%～25% of full range; Get each 20 μ l of need testing solution and contrast solution more respectively and inject liquid chromatograph, 2 times of record color atlas to principal constituent peak RT, in the need testing solution color atlas each impurity peak area with must not be greater than contrast solution main peak area (0.5%).
The 3-aminopropanol is got the about 1.0g of these article, and accurate the title decides, in the 50ml Erlenmeyer flask; After adding water 10ml dissolving; Shake up, add 2 of bromothymol blue indicating liquids, with sulfuric acid vs (0.01mol/L) titration to the solution displaing yellow; Every 1ml sulfuric acid vs (0.01mol/L) is equivalent to the aminopropanol of 0.75mg, must not cross 0.3%.
Moisture is got these article, measures according to aquametry (two appendix VIII of Chinese Pharmacopoeia version in 2005 M, the first method A), contains moisture and must not cross 0.5%.
Residue on ignition is got these article 1.0g, and inspection (two appendix VIII of Chinese Pharmacopoeia version in 2005 N) is left over residue and must not be crossed 0.1% in accordance with the law.
Heavy metal is got the residue of leaving under the residue on ignition item, and inspection (two appendix VIII of Chinese Pharmacopoeia version in 2005 H, second method) contains heavy metal and must not cross 10/1000000ths in accordance with the law.
[assay] got the about 0.4g of these article, and accurate the title decides, and puts in the 300ml flask; Precision adds perchloric acid vs (0.1mol/L) 50.0ml, refluxes cooling 5 hours; Notice preventing that moisture gets into from prolong in the air that clean prolong with the 5ml Glacial acetic acid min. 99.5, washing lotion is incorporated flask into; Add 5 of Viola crystallina indicating liquids, show blue-greenish colour with Potassium Hydrogen Phthalate solution titration to solution.And titrating result proofreaied and correct with blank test, every 1ml perchloric acid titration liquid (0.1mol/L) is equivalent to the C of 20.53mg
9H
19NO
4
The preparation precision of Potassium Hydrogen Phthalate solution takes by weighing the Potassium Hydrogen Phthalate of 20.42g in the 1000ml volumetric flask, adds warm the making fully of Glacial acetic acid min. 99.5 and dissolves, and notes avoiding the moisture absorption.Be cooled to room temperature, be diluted to scale, shake up with Glacial acetic acid min. 99.5.
The D-panthenol of preparation according to the invention is tested by above-mentioned quality controlling means, and each item quality control index all meets the requirements.
Embodiment
Following examples are just more specifically explained the present invention, and the present invention is not limited in the content of following examples.
Embodiment 1
Get D-(-)-pantoyl lactone 1.0kg, 3-amino-1-propyl alcohol 580g joins in the reactor drum, is heated to 50 ℃, the reaction 3h; Reduce to room temperature and promptly get the D-panthenol product, the stickiness liquid of clear and bright easy moisture absorption obtains finished product 1.58kg; Product yield 100%; Product is checked through above-mentioned quality controlling means, and each item quality control index is all up to specification, and specific optical rotation is+30.0 °.
Embodiment 2
Take by weighing D-(-)-pantoyl lactone of 3kg, add the reactor heating of 10L; Measure 6L ETHYLE ACETATE and add reactor drum, heated and stirred, the back of waiting to reflux adds gac 5g, decolours 30 minutes; Suction filtration, filtrating joins in the 25L container, adds sherwood oil 12L, mixes under back 5 ℃ and leaves standstill crystallization 2h; The suction filtration solid, 40 ℃ of vacuum-drying 2h of solid filtrate and reclaim then; Solid adds 5L ETHYLE ACETATE, stirs reflux down, adds gac 5g, decolours 30 minutes; Filter, filtrating joins in the 25L container, adds sherwood oil 10L, mixes under back 5 ℃ and leaves standstill crystallization 2h; Suction filtration, 40 ℃ of vacuum-dryings of solid got white solid 2.7kg yield 90% in 10 hours then.D-(-)-pantoyl lactone 1.0kg, the 3-amino-1-propyl alcohol 580g that get after making with extra care join in the reactor drum, are heated to 50 ℃, reaction 3h; Reduce to room temperature and promptly get the D-panthenol product, the stickiness liquid of clear and bright colourless easy moisture absorption obtains finished product 1.58kg; Total yield of products 90%; Product is checked through above-mentioned quality controlling means, and each item quality control index is all up to specification, and specific optical rotation is+30.8 °.
Embodiment 3
Take by weighing D-(-)-pantoyl lactone of 3kg, add the reactor heating of 10L; Measure 6L acetone and add reactor drum, heated and stirred, the back of waiting to reflux adds gac 5g, decolours 30 minutes; Suction filtration, filtrating joins in the 25L container, adds sherwood oil 12L, mixes under back 5 ℃ and leaves standstill crystallization 2h; Suction filtration solid, 40 ℃ of vacuum-drying 2h of solid then; Solid adds 5L acetone, stirs reflux down, adds gac 5g, decolours 30 minutes; Filter, filtrating joins in the 25L container, adds sherwood oil 10L, mixes under back 5 ℃ and leaves standstill crystallization 2h; Suction filtration, 40 ℃ of vacuum-dryings of solid obtained white solid 2.6kg, yield 87% in 10 hours then.D-(-)-pantoyl lactone 1.0kg, the 3-amino-1-propyl alcohol 580g that get after making with extra care join in the reactor drum, are heated to 60 ℃, reaction 3h.Reduce to room temperature and promptly get the D-panthenol product, the stickiness liquid of clear and bright colourless easy moisture absorption obtains finished product 1.58kg, total yield of products 87%, and product is checked through above-mentioned quality controlling means, and each item quality control index is all up to specification, and specific optical rotation is+30.6 °.
Embodiment 4
Take by weighing D-(-)-pantoyl lactone of 3kg, add the reactor heating of 10L; Measure 6L ETHYLE ACETATE and add reactor drum, heated and stirred, the back of waiting to reflux adds gac 5g, decolours 30 minutes; Suction filtration, filtrating joins in the 25L container, adds normal hexane 12L, mixes under back 5 ℃ and leaves standstill crystallization 2h; The suction filtration solid, 40 ℃ of vacuum-drying 2h of solid filtrate and reclaim then; Solid adds 5L ETHYLE ACETATE, stirs reflux down, adds gac 5g, decolours 30 minutes; Filter, filtrating joins in the 25L container, adds normal hexane 10L, mixes under back 5 ℃ and leaves standstill crystallization 2h; Suction filtration, 40 ℃ of vacuum-dryings of solid got white solid 2.6kg, yield 87% in 10 hours then.D-(-)-pantoyl lactone 1.0kg and the 3-amino-1-propyl alcohol 580g that get after making with extra care join in the reactor drum, are heated to 60 ℃, reaction 3h.Reduce to room temperature and promptly get the D-panthenol product, the stickiness liquid of clear and bright colourless easy moisture absorption obtains product 1.58kg, total yield of products 87%, and product is checked through above-mentioned quality controlling means, and each item quality control index is all up to specification, and specific optical rotation is+30.8 °.
Embodiment 5
Take by weighing D-(-)-pantoyl lactone of 3kg, add the reactor heating of 10L; Measure the 6L methylene dichloride and add reactor drum, heated and stirred, the back of waiting to reflux adds gac 5g, decolours 30 minutes; Suction filtration, filtrating joins in the 25L container, adds normal hexane 12L, mixes under back 5 ℃ and leaves standstill crystallization 2h; The suction filtration solid, 40 ℃ of vacuum-drying 2h of solid filtrate and reclaim then; Solid adds the 5L methylene dichloride, stirs reflux down, adds gac 5g, decolours 30 minutes; Filter, filtrating joins in the 25L container, adds normal hexane 10L, mixes under back 5 ℃ and leaves standstill crystallization 2h; Suction filtration, 40 ℃ of vacuum-dryings of solid got white solid 2.5kg, yield 83% in 10 hours then.D-(-)-pantoyl lactone 1.0kg and the 3-amino-1-propyl alcohol 580g that get after making with extra care join in the reactor drum, are heated to 60 ℃, reaction 3h.Reduce to room temperature and promptly get the D-panthenol product, the stickiness liquid of clear and bright colourless easy moisture absorption obtains product 1.58kg, total yield of products 83%, and product is checked through above-mentioned quality controlling means, and each item quality control index is all up to specification, and specific optical rotation is+30.5 °.
Embodiment 6
Take by weighing D-(-)-pantoyl lactone of 3kg, add the reactor heating of 10L; Measure the 6L methylene dichloride and add reactor drum, heated and stirred, the back of waiting to reflux adds gac 5g, decolours 30 minutes; Suction filtration, filtrating joins in the 25L container, adds hexanaphthene 12L, mixes under back 5 ℃ and leaves standstill crystallization 2h; The suction filtration solid, 40 ℃ of vacuum-drying 2h of solid filtrate and reclaim then; Solid adds the 5L methylene dichloride, stirs reflux down, adds gac 5g, decolours 30 minutes; Filter, filtrating joins in the 25L container, adds hexanaphthene 10L, mixes under back 5 ℃ and leaves standstill crystallization 2h; Suction filtration, 40 ℃ of vacuum-dryings of solid got white solid 2.5kg, yield 83% in 10 hours then.D-(-)-pantoyl lactone 1.0kg and the 3-amino-1-propyl alcohol 580g that get after making with extra care join in the reactor drum, are heated to 60 ℃, reaction 3h.Reduce to room temperature and promptly get the D-panthenol product, the stickiness liquid of clear and bright colourless easy moisture absorption obtains product 1.58kg, total yield of products 83%, and product is checked through above-mentioned quality controlling means, and each item quality control index is all up to specification, and specific optical rotation is+30.6 °.
Embodiment 7
Take by weighing D-(-)-pantoyl lactone of 3kg, add the reactor heating of 10L; Measure 6L ETHYLE ACETATE and add reactor drum, heated and stirred, the back of waiting to reflux adds gac 20g, decolours 30 minutes; Suction filtration, filtrating joins in the 25L container, adds sherwood oil 12L, mixes under back 5 ℃ and leaves standstill crystallization 2h; The suction filtration solid, 40 ℃ of vacuum-drying 2h of solid filtrate and reclaim then; Solid adds 5L ETHYLE ACETATE, stirs reflux down, adds gac 20g, decolours 30 minutes; Filter, filtrating joins in the 25L container, adds sherwood oil 10L, mixes under back 5 ℃ and leaves standstill crystallization 2h; Suction filtration, 40 ℃ of vacuum-dryings of solid got white solid 2.5kg yield 83% in 10 hours then.D-(-)-pantoyl lactone 1.0kg, the 3-amino-1-propyl alcohol 580g that get after making with extra care join in the reactor drum, are heated to 50 ℃, reaction 3h; Reduce to room temperature and promptly get the D-panthenol product, the stickiness liquid of clear and bright colourless easy moisture absorption obtains finished product 1.58kg; Total yield of products 83%; Product is checked through above-mentioned quality controlling means, and each item quality control index is all up to specification, and specific optical rotation is+30.3 °.
Embodiment 8
Take by weighing D-(-)-pantoyl lactone of 3kg, add the reactor heating of 10L; Measure 6L ETHYLE ACETATE and add reactor drum, heated and stirred, the back of waiting to reflux adds gac 1g, decolours 30 minutes; Suction filtration, filtrating joins in the 25L container, adds sherwood oil 12L, mixes under back 5 ℃ and leaves standstill crystallization 2h; The suction filtration solid, 40 ℃ of vacuum-drying 2h of solid filtrate and reclaim then; Solid adds 5L ETHYLE ACETATE, stirs reflux down, adds gac 1g, decolours 30 minutes; Filter, filtrating joins in the 25L container, adds sherwood oil 10L, mixes under back 5 ℃ and leaves standstill crystallization 2h; Suction filtration, 40 ℃ of vacuum-dryings of solid got white solid 2.7kg yield 90% in 10 hours then.D-(-)-pantoyl lactone 1.0kg, the 3-amino-1-propyl alcohol 580g that get after making with extra care join in the reactor drum, are heated to 50 ℃, reaction 3h; Reduce to room temperature and promptly get the D-panthenol product, the stickiness liquid of clear and bright colourless easy moisture absorption obtains finished product 1.58kg; Total yield of products 90%; Product is checked through above-mentioned quality controlling means, and each item quality control index is all up to specification, and specific optical rotation is+30.5 °.
Embodiment 9
Take by weighing D-(-)-pantoyl lactone of 3kg, add the reactor heating of 10L; Measure 6L ETHYLE ACETATE and add reactor drum, heated and stirred, the back of waiting to reflux adds gac 5g, decolours 30 minutes; Suction filtration, filtrating joins in the 25L container, adds sherwood oil 12L, mixes under back 5 ℃ and leaves standstill crystallization 2h; The suction filtration solid, 40 ℃ of vacuum-dryings of solid got white solid 2.8kg yield 93% in 10 hours then.D-(-)-pantoyl lactone 1.0kg, the 3-amino-1-propyl alcohol 580g that get after making with extra care join in the reactor drum, are heated to 50 ℃, reaction 3h; Reduce to room temperature and promptly get the D-panthenol product, the stickiness liquid of clear and bright colourless easy moisture absorption obtains finished product 1.58kg; Total yield of products 93%; Product is checked through above-mentioned quality controlling means, and each item quality control index is all up to specification, and specific optical rotation is+30.2 °.
Embodiment 10
Take by weighing D-(-)-pantoyl lactone of 3kg, add the reactor heating of 10L; Measure 6L acetone and add reactor drum, heated and stirred, the back of waiting to reflux adds gac 5g, decolours 30 minutes; Suction filtration, filtrating joins in the 25L container, adds sherwood oil 12L, mixes under back 5 ℃ and leaves standstill crystallization 2h; The suction filtration solid, 40 ℃ of vacuum-dryings of solid got white solid 2.8kg yield 93% in 10 hours then.D-(-)-pantoyl lactone 1.0kg, the 3-amino-1-propyl alcohol 580g that get after making with extra care join in the reactor drum, are heated to 50 ℃, reaction 3h; Reduce to room temperature and promptly get the D-panthenol product, the stickiness liquid of clear and bright colourless easy moisture absorption obtains finished product 1.58kg; Total yield of products 93%; Product is checked through above-mentioned quality controlling means, and each item quality control index is all up to specification, and specific optical rotation is+30.2 °.
Embodiment 11
Get D-(-)-pantoyl lactone 1.0kg, 3-amino-1-propyl alcohol 580g joins in the reactor drum, measures 6L ethanol and adds in the reactor drum, is heated to 50 ℃, reaction 3h; Add gac 1g, decoloured 30 minutes, suction filtration, filtrate decompression concentrates removes ethanol; Get the stickiness liquid of faint yellow easy moisture absorption, obtain finished product 1.58kg, product yield 100%; Product is checked through above-mentioned quality controlling means, and specific optical rotation is+29.1 °, 3-aminopropanol 0.9%.
Claims (12)
1. the preparation method of a D-panthenol is characterized in that D-(-)-pantoyl lactone and 3-amino-1-propyl alcohol reacts under solvent-free condition, obtains D-panthenol, and temperature of reaction is 40 ℃～100 ℃.
2. the preparation method of D-panthenol as claimed in claim 1 is characterized in that temperature of reaction is 50 ℃～70 ℃.
3. the preparation method of D-panthenol as claimed in claim 1 is characterized in that D-(-)-pantoyl lactone makes with extra care in advance, process for refining be D-(-)-pantoyl lactone through dissolution with solvents, and solvent crystallization purifying behind the activated carbon decolorizing.
4. the preparation method of D-panthenol as claimed in claim 3, the solvent that it is characterized in that dissolving D-(-)-pantoyl lactone is ETHYLE ACETATE, methylene dichloride, trichloromethane, acetone, methyl acetate.
5. the preparation method of D-panthenol as claimed in claim 4, the solvent that it is characterized in that dissolving D-(-)-pantoyl lactone is an ETHYLE ACETATE.
6. the preparation method of D-panthenol as claimed in claim 3 is characterized in that the crystallization purification solvent is sherwood oil, hexanaphthene, normal heptane, normal hexane alkane solvent.
7. the preparation method of D-panthenol as claimed in claim 6 is characterized in that the crystallization purification solvent is a sherwood oil.
8. the preparation method of D-panthenol as claimed in claim 3 is characterized in that D-(-)-pantoyl lactone and the mass/volume ratio of the solvent of dissolving D-(-)-pantoyl lactone are 1: 1 to 1: 4.
9. the preparation method of D-panthenol as claimed in claim 8 is characterized in that D-(-)-pantoyl lactone and the mass/volume ratio of the solvent of dissolving D-(-)-pantoyl lactone are 1: 2.
10. the preparation method of D-panthenol as claimed in claim 3 is characterized in that D-(-)-pantoyl lactone and the mass/volume ratio of crystallization purification solvent are 1: 1 to 1: 8.
11. the preparation method of D-panthenol as claimed in claim 10 is characterized in that D-(-)-pantoyl lactone and the mass/volume ratio of crystallization purification solvent are 1: 4.
12. the preparation method of D-panthenol as claimed in claim 3 is characterized in that the decoloration active carbon consumption is 0.01%～0.5% (w/v).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022219173A1 (en) * | 2021-04-15 | 2022-10-20 | Dsm Ip Assets B.V. | Production of panthenol |
| EP4108654A1 (en) * | 2021-06-23 | 2022-12-28 | DSM IP Assets B.V. | Production of panthenol |
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