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Solvent treatment method in chlorination technique in GCLE (7-phenylacetamido-3-cephem-4-carboxylic p-methoxybenzyl ester) synthesis process

A treatment method and solvent technology, which is applied in the field of solvent treatment in the chlorination process in the synthesis of GCLE, can solve the problems of high water recovery from solvents and cannot meet the requirements of reproduction, etc., and achieve the effects of reducing environmental pollution, facilitating promotion and application, and simple operation

Inactive Publication Date: 2016-05-11
TIANJIN PHARMA GROUP GENCOM PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the high moisture recovery of the solvent in the chlorination process in the synthesis of GCLE at present, which cannot meet the requirements of reproduction, in order to further process the solvent, the present invention provides a solvent treatment method in the chlorination process of the synthesis of GCLE, mainly using a desiccant Cooperate with distillation and azeotropic distillation to remove the moisture in the solvent, so that the recovered solvent can meet the requirements of reuse

Method used

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  • Solvent treatment method in chlorination technique in GCLE (7-phenylacetamido-3-cephem-4-carboxylic p-methoxybenzyl ester) synthesis process

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Effect test

Embodiment 1

[0014] The moisture of the solvent to be recovered is 4.33%. After the reaction, 300ml of the solvent to be recovered is taken and put into a reaction flask. In the solvent, add calcium oxide (CaO) and account for 1% of the recovered solvent. Calcium chloride (CaCl 2 ), heated to reflux for 3h and distilled at atmospheric pressure, collected cuts when the temperature was 101°C, collected 221ml of cuts altogether, and the recovery rate was 88.4%. After the treatment, the solvent moisture was 0.66%, and the moisture content was lower than 1.0%. Take advantage again.

Embodiment 2

[0016] The moisture content of the solvent to be recovered is 4.33%. Take 250mL of solvent and put it into a reaction bottle, install a 50mL water separator, heat and reflux to separate water for 3.0h, the reflux temperature is lower than 90°C, and reflux until no water drops fall. Separate the water layer 13mL, at this time the solvent moisture in the bottle is 1.25%, add 2.5g (about 1%) CaCl in the bottle 2 , stirred at room temperature for 30min, CaCl 2 It was lumped, and 215mL was obtained by filtration, the recovery rate was 86.0%, the water content after treatment was 0.69%, and the water content was lower than 1.0%, which belonged to the qualified category and could be reused.

Embodiment 3

[0018] The water content of the solvent to be recovered is 4.33%. Take 1000mL of solvent and put it into a bottle, install a 50mL water separator, heat and reflux to separate water, and stop when no water drops fall for about 2.5h. Separate the water layer 52mL, at this moment the solvent moisture in the bottle is 1.88%, add 10.0g (about 1%) CaCl in the bottle 2 , stirred at room temperature for 30min, CaCl 2 It was powdered and layered, and 834mL of solvent was obtained by filtration, with a recovery rate of 83.4%. After treatment, the water content was 0.79%, and the water content was lower than 1.0%, which was qualified and could be reused.

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Abstract

The invention provides a solvent treatment method in a chlorination technique in a GCLE (7-phenylacetamido-3-cephem-4-carboxylic p-methoxybenzyl ester) synthesis process. The method specifically comprises the following operation steps: putting a solvent to be recovered after reaction into a reaction bulb, installing a 50mL water separator, and heating under reflux to implement water separation until no water drops fall off, separating out the water layer, detecting the water content of the recovered solvent in the bulb at this time, adding calcium chloride which accounts for 1% of the recovered solvent into the bulb, stirring at normal temperature until the calcium chloride becomes powdery and stratified, and filtering to obtain the recovered solvent, wherein the water content in the treated solvent is 0.66-0.69%. The method can also comprises the following steps: adding drying agents calcium oxide and calcium chloride instead of the water separator treatment to recover the treated solvent, and carrying out atmospheric distillation on the treated solvent to obtain the fraction to be recovered. The method provided by the invention is simple to operate, has high repetitiveness, and is convenient for popularization and application.

Description

technical field [0001] The invention relates to a solvent treatment method in a medicine synthesis process, in particular to a solvent treatment method in a chlorination process in synthesizing GCLE. Background technique [0002] GCLE (7-phenylacetamido-3-chloromethyl cephalosporanic acid p-methoxybenzyl ester) was developed by Japan in the 1990s and is a new type of cephalosporin developed after 7-ACA and 7-ADCA antibiotic-like mother nucleus. GCLE can synthesize dozens of cephalosporin products, especially the third and fourth generation cephalosporin products, such as cefoperazone, ceftazidime, ceftriaxone, cefixime, cefepime, ceftibuten, etc. When GCLE is used as the mother nucleus to produce cephalosporins, the product yield is higher, the production process is simpler, the production conditions are milder, and the product cost is lower. The chlorination process of GCLE synthesis is as follows: [0003] [0004] The solvents used in the chlorination process are ma...

Claims

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Application Information

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IPC IPC(8): C07D319/12C07C7/00C07C15/06
CPCC07D319/12C07C7/005
Inventor 芮庆云赵君彦赵洪霞魏晨曦
Owner TIANJIN PHARMA GROUP GENCOM PHARMA
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