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Bromoacetyl-7-ACA production process

A technology of -7-ACA and 7-ACA, applied in the field of bromoacetyl-7-ACA production technology, can solve the problems of destroying reaction raw materials and incomplete reaction, achieve simple and easy operation process, improve product quality and product yield Yield effect

Pending Publication Date: 2020-08-28
佛山市南海北沙制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The neutralization process is partially alkaline, destroying the reaction raw materials, resulting in incomplete reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 2

[0047] Acetyl-7-ACA production process in the present embodiment is characterized in that, comprises the following steps:

[0048] S1. Add 1600ml of purified water and 80g of 7-ACA to the reaction bottle, and stir evenly;

[0049] S2. Adjust and keep the temperature of the material at 0-5°C, add 29g of triethylamine dropwise within 25-30 minutes, after the dropwise addition, stir for 5-15 minutes to completely dissolve the material;

[0050] S3. Add 10 g of activated carbon, stir and decolorize for 15 to 20 minutes;

[0051] S4. filter, get filtrate;

[0052] S5. Add 845ml of toluene and 44g of calcium salt, adjust and keep the material temperature at 13-20°C, and add 83g of bromoacetyl bromide dropwise within 30-60 minutes under rapid stirring;

[0053] S6. After the dropwise addition is completed, the temperature of the material is controlled at 18-20°C, and the reaction is stirred for 1-1.5 hours;

[0054] S7. after completion of the reaction, filter to filter out excess...

Embodiment 3

[0065] Acetyl-7-ACA production process in the present embodiment is characterized in that, comprises the following steps:

[0066] S1. Add 1650ml of purified water and 75g of 7-ACA to the reaction bottle, and stir evenly;

[0067] S2. Adjust and keep the temperature of the material at 0-5°C, add 28.5 g of triethylamine dropwise within 25-30 minutes, after the dropwise addition, stir for 5-15 minutes to completely dissolve the material;

[0068] S3. Add 10 g of activated carbon, stir and decolorize for 15 to 20 minutes;

[0069] S4. filter, get filtrate;

[0070] S5. Add 800ml of toluene and 40g of calcium salt, adjust and keep the material temperature at 13-20°C, and add 78g of bromoacetyl bromide dropwise within 30-60 minutes under rapid stirring;

[0071] S6. After the dropwise addition is completed, the temperature of the material is controlled at 18-20°C, and the reaction is stirred for 1-1.5 hours;

[0072] S7. after completion of the reaction, filter to filter out exc...

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PUM

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Abstract

The invention discloses a bromoacetyl-7-ACA production process which comprises the following steps: S1, adding purified water and 7-ACA into a reaction bottle, and uniformly stirring; S2, adjusting and keeping the temperature of the material at 0-5 DEG C, dropwise adding triethylamine within 25-30 minutes, and stirring until the solution is clear; S3, adding activated carbon, and stirring for decolorization for 15-20 minutes; S4, filtering, and taking filtrate; S5, adding methylbenzene and calcium salt, controlling the temperature of the materials to be 13-20 DEG C, accelerating the stirring speed, and dropwise adding bromoacetyl bromide within 30-60 minutes; S6, after the bromoacetyl bromide is dropwise added, controlling the temperature to be 18-20 DEG C, and stirring to react for 1-1.5hours; S7, filtering to remove excessive calcium salt; standing the filtrate for 1-2 hours, layering, taking the lower-layer liquid material, and recycling the upper layer for later use; S9, adding 95% ethanol into the lower-layer liquid material, keeping the temperature at 10-15 DEG C, and dropwise adding a hydrochloric acid solution until the pH value is 1.0; S10, reducing the stirring rotatingspeed, and maintaining the temperature and growing the crystal for 30 minutes; S11, filtering, and taking a filter cake; S12, washing the filter cake with purified water; S13, washing the filter cakewith ethanol; and S14, discharging, and drying the filter cake to obtain a finished product.

Description

technical field [0001] The invention relates to the technical field of pharmacy, in particular to a production process of bromoacetyl-7-ACA. Background technique [0002] Bromoacetyl-7-ACA is an intermediate of cefathiamidine. In the current synthesis process, sodium bicarbonate alkali solution is used as an acid-binding agent to neutralize acidic by-products during the reaction and keep the reaction solution neutral. The neutralization process is partially alkaline, destroying the reaction raw materials, resulting in incomplete reaction. Contents of the invention [0003] The purpose of the present invention is to overcome the deficiencies of the prior art and provide a production process for bromoacetyl-7-ACA. [0004] In order to achieve the above object, the technical solution adopted in the present invention is: [0005] A kind of bromoacetyl-7-ACA production technique is characterized in that, comprises the following steps: [0006] S1. Add purified water and 7-AC...

Claims

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Application Information

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IPC IPC(8): C07D501/06C07D501/12C07D501/28
CPCC07D501/06C07D501/12C07D501/28
Inventor 黄升黎小雄徐伟邱伟杰袁莉莉
Owner 佛山市南海北沙制药有限公司