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Preparing method of cis, trans-ethyl 2, 2-dimethyl-3-(1-isobutenyl)cyclopropane-1-carboxylate

A technology of ethyl cyclopropanecarboxylate and ethyl aminoacetate hydrochloride, which is applied to the preparation of carboxylate, the separation/purification of carboxylate, and the preparation of organic compounds, etc., can solve the problems of increasing processing costs and achieve The effect of convenient operation, high content and high product yield

Pending Publication Date: 2017-01-11
江苏优普生物化学科技股份有限公司
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AI Technical Summary

Problems solved by technology

Due to the excess of sodium nitrite and acid, these processes will inevitably produce nitrogen oxides, which will produce acidic wastewater after the reaction, increasing the cost of treatment

Method used

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Embodiment Construction

[0016] The 1000ml four-necked bottle is installed in a water bath, equipped with a stirring device, a bulb condenser, and a thermometer, and the condenser is connected to frozen brine. Add 100 grams of water and 170 grams of 98.5% ethyl aminoacetate hydrochloride into the four-neck bottle, stir and dissolve, add frozen brine to the water bath, cool down to 0°C~-2°C, and add 350 grams of dichloroethane. Add 78 grams of 98% sodium nitrite to a 500ml beaker, add 80 grams of water, stir to dissolve, and pour it into a 250ml constant pressure funnel. Connect the constant pressure funnel to the four-necked bottle, add sodium nitrite solution dropwise to the ethyl aminoacetate hydrochloride solution, adjust the dropping rate and brine temperature, control the reaction temperature at -2±2°C, and control the dropping time at 4- 6 hours. After the dropwise addition is completed, keep the temperature at -2±2°C until the discoloration is detected by starch potassium iodide, and the react...

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PUM

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Abstract

The invention discloses a method of preparing cis, trans-ethyl 2,2-dimethyl-3-(1-isobutenyl)cyclopropane-1-carboxylate, comprising of making the ethyl glycinate hydro and sodium nitrite in the solvent diazo-react without additional addition of organic acid or mineral acid to get ethyl diazoacetate which is to react with the 2,5-Dimethyl-2,4-hexadiene under the catalyst effect and then be desolvated and rectificated to get ethyl chrysanthemumate.The invention is easy to use with high production yield and high contents.

Description

technical field [0001] The invention relates to a preparation method of ethyl cis,trans-2,2-dimethyl-3-(2-methyl-1-propenyl)cyclopropanecarboxylate (namely ethyl chrysanthemum acid). Background technique [0002] Ethyl permethrin is the key intermediate of various pyrethroids such as resmethrin, allethrin, resmethrin, tetramethrin, methothrin, etc. The general synthesis route is to use ethyl aminoacetate hydrochloride Ethyl diazoacetate is obtained, and then synthesized by cyclization of ethyl diazoacetate and 2,5-dimethyl-2,4-hexadiene. [0003] Existing synthesis of ethyl diazoacetate generally carries out diazotization reaction with ethyl aminoacetate hydrochloride under acidic conditions and a slight excess of sodium nitrite. The acids used include dilute sulfuric acid, acetic acid, hydrochloric acid, etc., produced by Zhongshan Kaizhong Technique uses reactions in acetic acid-sodium acetate buffer. Due to the excess of sodium nitrite and acid, these processes will ine...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/343C07C67/48C07C69/747
CPCC07C67/343C07C67/48C07C245/20C07C69/747
Inventor 张继钱邹笑天于海军
Owner 江苏优普生物化学科技股份有限公司
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