CN105461584A - Compounding method of intermediate body, namely 2-chloro-N-phenyl-acetamide, of carcainium chloride medicine - Google Patents
Compounding method of intermediate body, namely 2-chloro-N-phenyl-acetamide, of carcainium chloride medicine Download PDFInfo
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- CN105461584A CN105461584A CN201510974125.9A CN201510974125A CN105461584A CN 105461584 A CN105461584 A CN 105461584A CN 201510974125 A CN201510974125 A CN 201510974125A CN 105461584 A CN105461584 A CN 105461584A
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- Prior art keywords
- chloroacetylaniline
- acetamide
- synthetic method
- carcainium chloride
- pharmaceutical intermediate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/08—Preparation of carboxylic acid amides from amides by reaction at nitrogen atoms of carboxamide groups
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a compounding method of an intermediate body, namely 2-chloro-N-phenyl-acetamide, of a carcainium chloride medicine. The compounding method comprises the following steps of adding 160 to 190 ml of oxalic acid in a reaction vessel which is provided with a stirrer, a reflux condenser and a thermometer; reducing the solution temperature to be 3 to 5 DEG C; slowly adding 0.29 mol of aniline (3); dripping 0.29 to 0.32 mol of chloroacetamide, and controlling the dripping time to be 50 to 70 minutes, the stirring speed to be 130 to 160 rpm and the stirring time to be 60 to 80 minutes; adding 200 ml of potassium carbonate solution; then continuously stirring for 80 to 90 minutes; filtering; washing a filter cake by using a saline solution until the pH (Potential of Hydrogen) is 6 to 7; dewatering by using a dewatering agent; obtaining 2-chloro-N-phenyl-acetamide, wherein the mass percentage of oxalic acid is 30 to 35 percent.
Description
Technical field
The present invention relates to a kind of synthetic method of carcainium chloride pharmaceutical intermediate N-chloroacetylaniline.
Background technology
Carcainium chloride medicine is a kind of cats product, belong to non oxidizing bactericide, there is wide spectrum, efficiently sterilization algae removal ability, effectively can control bacterium algae propagation and foundry loam growth in water, and there is good sludge stripping effect and certain dispersion, osmosis, there is certain ability of deoiling and corrosion inhibition simultaneously.This product has high sterilization algae removal ability, toxicity is little, water soluble, easy to use, do not affect by the water hardness, and there is strong stripping effect, be therefore specially adapted to Biocidal algae-killing agent and the ooze stripper of recirculated cooling water in large scale chemical plant, consumption 100ppm.Be dissociated into cationic reactive groups in aqueous, there is the effect of clean, sterilization only.Being widely used in the sterilization of skin and instruments when medical operating, being also widely used in the aspects such as sterilization, sterilization, anticorrosion, emulsification, de-sludging, solubilising, is again the levelling agent of cationic dyestuff dye acrylic fiber.N-chloroacetylaniline is as carcainium chloride pharmaceutical intermediate, and its synthetic method is good and bad for raising pharmaceutical synthesis quality product, reduces by-products content and has Important Economic meaning.
Summary of the invention
The object of the present invention is to provide a kind of synthetic method of carcainium chloride pharmaceutical intermediate N-chloroacetylaniline, comprise the steps:
I () is in the reaction vessel being provided with agitator, reflux exchanger, thermometer, add oxalic acid 160-190ml, reduce solution temperature to 3--5 DEG C, slowly add aniline (3) 0.29mol, drip chlor(o)acetamide 0.29-0.32mol, time for adding controls at 50-70min, control stirring velocity 130-160rpm, churning time 60-80min, adds solution of potassium carbonate 200ml, then continues stirring 80-90min, filter, filter cake brine is 6-7 to pH, and dewatering agent dewaters, and obtains N-chloroacetylaniline;
A synthetic method for carcainium chloride pharmaceutical intermediate N-chloroacetylaniline, the massfraction of the oxalic acid described in step (i) is 30-35%.
A synthetic method for carcainium chloride pharmaceutical intermediate N-chloroacetylaniline, the solution of potassium carbonate massfraction described in step (i) is 40-45%.
A synthetic method for carcainium chloride pharmaceutical intermediate N-chloroacetylaniline, the salts solution described in step (i) is any one in SODIUMNITRATE, Repone K.
A synthetic method for carcainium chloride pharmaceutical intermediate N-chloroacetylaniline, the dewatering agent described in step (i) is any one in anhydrous magnesium sulfate, solid sodium hydroxide.
Whole reaction process can represent with following reaction formula:
The invention has the advantages that: the middle-chain decreasing reaction, reduce temperature of reaction and reaction times, improve reaction yield.
Embodiment
Below in conjunction with concrete embodiment, the invention will be further described:
A kind of synthetic method of carcainium chloride pharmaceutical intermediate N-chloroacetylaniline
Example 1:
In the reaction vessel being provided with agitator, reflux exchanger, thermometer; adding massfraction is 32% oxalic acid 160ml; reduce solution temperature to 3 DEG C; slowly add aniline (3) 0.29mol; drip chlor(o)acetamide 0.29mol; time for adding controls at 50min; control stirring velocity 130rpm, churning time 60min, adding massfraction is 40% solution of potassium carbonate 200ml; continue again to stir 80min; filter, the washing of filter cake sodium nitrate solution is 6 to pH, and anhydrous magnesium sulfate dewaters; obtain N-chloroacetylaniline 38.45g, yield 78%.
Example 2:
I () is in the reaction vessel being provided with agitator, reflux exchanger, thermometer; adding massfraction is 32% oxalic acid 170ml; reduce solution temperature to 4 DEG C; slowly add aniline (3) 0.29mol; drip chlor(o)acetamide 0.31mol; time for adding controls at 60min; control stirring velocity 140rpm, churning time 70min, adding massfraction is 42% solution of potassium carbonate 200ml; continue again to stir 85min; filter, the washing of filter cake sodium nitrate solution is 7 to pH, and solid sodium hydroxide dewaters; obtain N-chloroacetylaniline 40.92g, yield 83%.
Example 3:
In the reaction vessel being provided with agitator, reflux exchanger, thermometer; adding massfraction is 35% oxalic acid 190ml; reduce solution temperature to 5 DEG C; slowly add aniline (3) 0.29mol; drip chlor(o)acetamide 0.32mol; time for adding controls at 70min; control stirring velocity 160rpm, churning time 60-80min, adding massfraction is 45% solution of potassium carbonate 200ml; continue again to stir 90min; filter, the washing of filter cake sodium nitrate solution is 7 to pH, and anhydrous magnesium sulfate dewaters; obtain N-chloroacetylaniline 42.40g, yield 86%.
Claims (4)
1. a synthetic method for carcainium chloride pharmaceutical intermediate N-chloroacetylaniline, is characterized in that, comprise the steps:
I () is in the reaction vessel being provided with agitator, reflux exchanger, thermometer, add oxalic acid 160-190ml, reduce solution temperature to 3--5 DEG C, slowly add aniline (3) 0.29mol, drip chlor(o)acetamide 0.29-0.32mol, time for adding controls at 50-70min, control stirring velocity 130-160rpm, churning time 60-80min, adds solution of potassium carbonate 200ml, then continues stirring 80-90min, filter, filter cake brine is 6-7 to pH, and dewatering agent dewaters, and obtains N-chloroacetylaniline; Wherein, the massfraction of the oxalic acid described in step (i) is 30-35%.
2. the synthetic method of a kind of carcainium chloride pharmaceutical intermediate N-chloroacetylaniline according to claim 1, it is characterized in that, the solution of potassium carbonate massfraction described in step (i) is 40-45%.
3. the synthetic method of a kind of carcainium chloride pharmaceutical intermediate N-chloroacetylaniline according to claim 1, is characterized in that, the salts solution described in step (i) is any one in SODIUMNITRATE, Repone K.
4. the synthetic method of a kind of carcainium chloride pharmaceutical intermediate N-chloroacetylaniline according to claim 1, is characterized in that, the dewatering agent described in step (i) is any one in anhydrous magnesium sulfate, solid sodium hydroxide.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510974125.9A CN105461584A (en) | 2015-12-23 | 2015-12-23 | Compounding method of intermediate body, namely 2-chloro-N-phenyl-acetamide, of carcainium chloride medicine |
| CN201610813977.4A CN106397246A (en) | 2015-12-23 | 2016-09-11 | Compounding method of intermediate body, namely 2-chloro-N-phenyl-acetamide, of carcainium chloride medicine |
| AU2016102186A AU2016102186A4 (en) | 2015-12-23 | 2016-12-22 | Carcainium chloride drug intermediates N-chloroacetyl-aniline synthesis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510974125.9A CN105461584A (en) | 2015-12-23 | 2015-12-23 | Compounding method of intermediate body, namely 2-chloro-N-phenyl-acetamide, of carcainium chloride medicine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105461584A true CN105461584A (en) | 2016-04-06 |
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Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510974125.9A Pending CN105461584A (en) | 2015-12-23 | 2015-12-23 | Compounding method of intermediate body, namely 2-chloro-N-phenyl-acetamide, of carcainium chloride medicine |
| CN201610813977.4A Pending CN106397246A (en) | 2015-12-23 | 2016-09-11 | Compounding method of intermediate body, namely 2-chloro-N-phenyl-acetamide, of carcainium chloride medicine |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610813977.4A Pending CN106397246A (en) | 2015-12-23 | 2016-09-11 | Compounding method of intermediate body, namely 2-chloro-N-phenyl-acetamide, of carcainium chloride medicine |
Country Status (1)
| Country | Link |
|---|---|
| CN (2) | CN105461584A (en) |
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2015
- 2015-12-23 CN CN201510974125.9A patent/CN105461584A/en active Pending
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2016
- 2016-09-11 CN CN201610813977.4A patent/CN106397246A/en active Pending
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| CN106397246A (en) | 2017-02-15 |
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Application publication date: 20160406 |