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Method for improving N-(4-methoxyphenyl)-4-acetyl-3-(1-hydroxyl)ethylazetidinone-2 synthesis conversion rate

A technology of methoxybenzene and heterocyclobutanone, which is applied in the field of medicine and chemical industry, can solve the problems of production accidents, difficulty in wastewater treatment, large amount of catalyst, etc., and achieve small solid waste generation, clear layered interface, and rapid reaction The effect of shortening the time

Inactive Publication Date: 2014-11-05
JIANGSU RUIKE MEDICAL SCI & TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The amount of catalyst is large, and the interface is difficult to distinguish during extraction, the controllability of the operation is poor, material running is easy to occur, and production accidents occur. There is a lot of solid waste in the wastewater, which makes wastewater treatment difficult.

Method used

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  • Method for improving N-(4-methoxyphenyl)-4-acetyl-3-(1-hydroxyl)ethylazetidinone-2 synthesis conversion rate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Under the protection of nitrogen, add tri-n-butylamine and dichloromethane in turn, control the temperature at about -30°C, add 220g of tetraisopropyloxytitanium dropwise, and dropwise add step-by-step at -30±5°C The obtained amide solution (containing about 0.75 mol of acylate) was added dropwise and kept at -30±5° C. for 5 hours. The reaction solution was added with 31% hydrochloric acid in an equimolar amount to the amide, and the dropping temperature was controlled at -5° C. Stir the feed solution for 30 minutes, let it stand, and separate layers. The acid water layer goes to waste water treatment, and the organic layer is added with 31% hydrochloric acid in an equimolar amount to the amide for the second pickling, static layering, and the acid water goes to waste water treatment. The layer is transferred to the washing pot, then add 100g baking soda and 50g water for alkali washing, stir for 1 hour, let stand for 1 hour, separate layers, remove the water layer for w...

Embodiment 2

[0019] Under the protection of nitrogen, add tri-n-butylamine and dichloromethane in turn, control the temperature at about -30°C, add 240g of tetraisopropyloxytitanium dropwise, and after the addition is completed, add step-by-step at -30±5°C The obtained amide solution (containing about 0.75 mol of acylate) was added dropwise and kept at -30±5° C. for 5 hours. The reaction solution was added with 31% hydrochloric acid in an equimolar amount to the amide, and the dropping temperature was controlled at -5° C. Stir the feed solution for 30 minutes, let it stand, and separate layers. The acid water layer goes to waste water treatment, and the organic layer is added with 31% hydrochloric acid in an equimolar amount to the amide for the second pickling, static layering, and the acid water goes to waste water treatment. The layer is transferred to the washing pot, then add 100g baking soda and 50g water for alkali washing, stir for 1 hour, let stand for 1 hour, separate layers, remo...

Embodiment 3

[0021] Under the protection of nitrogen, add tri-n-butylamine and dichloromethane in turn, control the temperature at about -30°C, add 260g of tetraisopropyloxytitanium dropwise, after the dropwise addition, at -30±5°C, add step by step The obtained amide solution (containing about 0.75 mol of acylate) was added dropwise and kept at -30±5° C. for 5 hours. The reaction solution was added with 31% hydrochloric acid in an equimolar amount to the amide, and the dropping temperature was controlled at -5° C. Stir the feed solution for 30 minutes, let it stand, and separate layers. The acid water layer goes to waste water treatment, and the organic layer is added with 31% hydrochloric acid in an equimolar amount to the amide for the second pickling, static layering, and the acid water goes to waste water treatment. The layer is transferred to the washing pot, then add 100g baking soda and 50g water for alkali washing, stir for 1 hour, let stand for 1 hour, separate layers, remove the ...

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Abstract

A disclosed method for improving N-(4-methoxyphenyl)-4-acetyl-3-(1-hydroxyl)ethylazetidinone-2 synthesis conversion rate comprises: under the protection of nitrogen, successively adding tri-n-butylamine and dichloromethane, controlling the temperature at -35 DEG C to -25 DEG C, adding titanium tetraisopropanolate, then adding an amide solution at -35 DEG C to -25 DEG C and keeping warm for 5 h, adding hydrochloric acid with the mass percent of 31% and the molar quantity equal to that of the amide into the reaction solution, controlling the temperature at -5 DEG C, stirring the material solution for 30 min, standing, layering, performing wastewater removing processing on the acidic water layer, and again adding hydrochloric acid with the mass percent of 31% and the molar quantity equal to that of the amide into the organic layer for secondary acid cleaning, standing and layering, performing wastewater removing processing on the acidic water layer, transferring the organic layer to a washing pan, then adding sodium bicarbonate and water for base cleaning, stirring for 1 h, standing for 1 h, layering, performing wastewater removing processing on the water layer, performing reduced-pressure distillation on the organic layer, concentrating to obtain a solid, then adding DMF to dissolve for direct next-step usage. According to the method, the reaction time is shortened, and the main reaction conversion rate is improved by 10-13%.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and specifically relates to a method for increasing the concentration of carbapenicillin intermediate N-(4-methoxybenzene)-4-acetyl-3-[1-(tert-butyldimethylsilyloxy)ethyl Base] azetidinone-2 conversion method. Background technique [0002] Synthesis of carbapenicillin intermediate N-(4-methoxybenzene)-4-acetyl-3-(1-hydroxyl)ethylazetidinone-2, the original process uses aluminum chloride as catalyst, dosage 4 molar ratios of main raw materials. The amount of catalyst is large, and the interface is difficult to distinguish during extraction, the controllability of the operation is poor, it is easy to cause material run-off, resulting in production accidents, and there is a lot of solid waste in the wastewater, which makes wastewater treatment difficult. Contents of the invention [0003] The purpose of this section is to outline some aspects of embodiments of the invention and brie...

Claims

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Application Information

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IPC IPC(8): C07D205/08
CPCC07D205/08
Inventor 赵小泉陆华朱家伍何蒲军匡立幸
Owner JIANGSU RUIKE MEDICAL SCI & TECH CO LTD
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