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A kind of technology that straight-through method prepares ampicillin

A technology for preparing ampicillin and ampicillin, applied in the field of pharmaceutical preparation, can solve the problem of high cost and achieve the effects of high conversion rate, increased yield and increased profit

Active Publication Date: 2017-12-12
INNER MONGOLIA CHANGSHENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this patent requires post-processing procedures such as separation and drying of phenylglycine methyl ester hydrochloride, so the cost is relatively high

Method used

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  • A kind of technology that straight-through method prepares ampicillin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1 Straight-through method prepares ampicillin

[0018] (1) Dissolve 0.4mol L-phenylglycine in 4.8mol anhydrous methanol, add thionyl chloride dropwise under ice-water bath cooling and stir, wherein, the molar ratio of L-phenylglycine, anhydrous methanol and thionyl chloride is 1 :12:1; after the dropwise addition of thionyl chloride, heat and reflux in a 65°C water bath for 1.8h, the rate of dropping thionyl chloride is 4mL / min; when the purity of phenylglycine methyl ester hydrochloride is ≥97%, Stop the reaction, distill the unreacted methanol under reduced pressure at a temperature of 60°C and a vacuum of ≥0.070Mp, add water to the obtained white solid until the water is dissolved and clear, then adjust the pH to 3.0 with 10% ammonia water, The solution of L-phenylglycine methyl ester hydrochloride was obtained;

[0019] (2) 0.36mol6-APA is dissolved in water and adjusted to pH 8.0 with 10% ammonia water to clarify the solution, and put into the reactor t...

Embodiment 2

[0021] Embodiment 2 Straight-through method prepares ampicillin

[0022] (1) Dissolve 0.4mol L-phenylglycine in 4.0mol anhydrous methanol, add thionyl chloride dropwise under ice-water bath cooling and stir, wherein, the molar ratio of L-phenylglycine, anhydrous methanol and thionyl chloride is 1 :10:1; after the dropwise addition of thionyl chloride, heat and reflux in a 65°C water bath for 1.5h, and dropwise add thionyl chloride at a speed of 3mL / min; when the purity of phenylglycine methyl ester hydrochloride is ≥97%, Stop the reaction, distill the unreacted methanol under reduced pressure at a temperature of 55°C and a vacuum degree of ≥0.070Mp, add water to the obtained white solid until the water is dissolved and clear, adjust the pH to 2.0 with 5% ammonia water, The solution of L-phenylglycine methyl ester hydrochloride was obtained;

[0023] (2) 0.37mol6-APA is dissolved in water and adjusted to pH 7.5 with 5% ammonia water to clarify the solution, and put into the re...

Embodiment 3

[0025] Embodiment 3 Straight-through method prepares ampicillin

[0026] (1) Dissolve 0.4mol L-phenylglycine in 5.6mol anhydrous methanol, add thionyl chloride dropwise under ice-water bath cooling and stir, wherein, the molar ratio of L-phenylglycine, anhydrous methanol and thionyl chloride is 1 :14:1; after the dropwise addition of thionyl chloride, heat and reflux in a 65°C water bath for 1.5h, and the rate of dropping thionyl chloride is 5mL / min; when the purity of phenylglycine methyl ester hydrochloride is ≥97%, Stop the reaction, distill the unreacted methanol under reduced pressure at a temperature of 65°C and a vacuum of ≥0.070Mp, add water to the obtained white solid until the water is dissolved and clear, then adjust the pH to 4.0 with 15% ammonia water, The solution of L-phenylglycine methyl ester hydrochloride was obtained;

[0027] (2) 0.34mol6-APA is dissolved in water and adjusted to pH 8.5 with 15% ammonia water to clarify the solution, and put into the react...

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Abstract

The invention relates to a process for preparing ampicillin by a straight-through method, belonging to the technical field of medicine preparation. This process uses phenylglycine as the starting material to finally synthesize ampicillin. Compared with chemical methods and other enzymatic methods, it saves steps such as subsequent drying of phenylglycine methyl ester hydrochloride, which significantly increases the yield and reduces the The investment in fixed assets reduces energy loss, equipment loss, reduces costs, improves efficiency, and increases profits. It is worth promoting in production.

Description

technical field [0001] The invention relates to a process for preparing ampicillin, in particular to a process for preparing ampicillin by a straight-through method, and belongs to the technical field of medicine preparation. Background technique [0002] Ampicillin is an important β-lactam antibiotic with a broad antibacterial spectrum and has inhibitory effects on both Gram-negative and positive bacteria. It has a strong effect and is widely used in clinical practice. Ampicillin can also synthesize semi-synthetic penicillin ampicillin sodium, mezlocillin and so on. [0003] At present, the synthetic method of ampicillin has two kinds of processes of chemical method and enzymatic method. The technological process of the chemical method is as follows: after mixing the potassium salt of phenylglycine and pivaloyl chloride, ampicillin is finally prepared through processes such as mixing anhydride, condensation, hydrolysis, and crystallization. The process involves a large a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C12P37/04
Inventor 陈顺记郭建明陈英新韩贺东王继明王秋红刘晓艳
Owner INNER MONGOLIA CHANGSHENG PHARMA
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