Preparation method of ethyl 6-oxo-8-chloro-caprylate

A technology of ethyl chlorooctanoate and ethyl hexanoate, which is applied in the field of preparation of lipoic acid intermediates, can solve the problems of increased wastewater volume and low cooling efficiency, and achieve reduced wastewater volume, high cooling efficiency, and good industrial application value effect

A technology of ethyl chlorooctanoate and ethyl hexanoate, which is applied in the field of preparation of lipoic acid intermediates, can solve the problems of increased wastewater volume and low cooling efficiency, and achieve reduced wastewater volume, high cooling efficiency, and good industrial application value effect

CN102731307AActive Publication Date: 2012-10-17JIANGSU TOHOPE PHARMA
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  • Preparation method of ethyl 6-oxo-8-chloro-caprylate
  • Preparation method of ethyl 6-oxo-8-chloro-caprylate
  • Preparation method of ethyl 6-oxo-8-chloro-caprylate

Examples

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Effect test

Embodiment 1

[0032] 4000kg of water into 10M 3 In the hydrolysis kettle, ice salt water is passed into the jacket of the hydrolysis kettle. The hydrolysis kettle is equipped with a circulation pump and a circulation pipeline. The circulation pipeline is connected to a graphite condenser. Brine, the material is cooled and then recycled back to the hydrolysis tank. Use a jacket and a graphite condenser to circulate and cool the water in the hydrolysis tank to below 10°C for later use.

[0033] Add 1280Kg of dichloroethane into a 1500L reaction kettle, add 450Kg of aluminum trichloride, stir, cool down to 10°C-18°C with an ice-salt water jacket, add dropwise 360kg of ethyl 6-chloro-6-oxohexanoate, and Control the temperature at 20°C to 25°C, and pass through ethylene for 3 hours to obtain the addition reaction solution. Put the reaction liquid into the spare 4000kg water in the hydrolysis kettle, stir it, and then enter the graphite condenser through the circulation pump to cool it, then re...

Embodiment 2

[0036] 4000kg of water into 10M 3 In the hydrolysis kettle, ice salt water is passed into the jacket of the hydrolysis kettle. The hydrolysis kettle is equipped with a circulation pump and a circulation pipeline. The circulation pipeline is connected to a graphite condenser. Brine, the material is cooled and then recycled back to the hydrolysis tank. Cool with jacket ice brine and graphite condenser ice brine, cool down to below 10°C by circulation, and set aside.

[0037] Add 1280Kg of dichloroethane into a 1500L reaction kettle, add 450Kg of aluminum trichloride, stir, cool down to 10°C-18°C with an ice-salt water jacket, add dropwise 360kg of ethyl 6-chloro-6-oxohexanoate, and Control the temperature at 20°C to 25°C, and pass through ethylene for 3 hours to obtain the addition reaction solution. Put the reaction liquid into the spare 4000kg water in the hydrolysis kettle, stir it, and then enter the graphite condenser through the circulation pump to cool it, then return i...

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Abstract

The invention relates to a preparation method of ethyl 6-oxo-8-chloro-caprylate, which comprises the steps of: carrying out addition reaction on ethyl 6-chloro-6-oxo-caproate and ethylene in dichloroethane solution with aluminum trichloride as a catalyst; mixing the addition reaction liquid with water in a hydrolysis kettle; introducing the mixture of the reaction liquid and water into a graphite condenser for cooling through a circulating pump; returning to the hydrolysis kettle; and continuously circulating until hydrolysis is finished. The method solves the technical problems caused by hydrolysis of the addition product, effectively controls the hydrolysis reaction temperature, shortens the hydrolysis reaction time, increases the reaction yield by about 10% and saves the water consumed by the hydrolysis reaction by 50%.

Description

technical field [0001] The invention relates to a preparation method of a lipoic acid intermediate, in particular to a preparation method of 6-oxo-8-chlorooctanoic acid ethyl ester. Background technique [0002] 6-oxo-8-chlorooctanoic acid ethyl ester, whose structure is shown in the following formula, is a chemical reaction intermediate for the synthesis of 6,8-dichlorooctanoic acid ethyl ester, and 6,8-dichlorooctanoic acid ethyl ester It is an important intermediate in the synthesis of lipoic acid. [0003] [0004] One of the synthetic methods of lipoic acid is to use adipic acid as the starting material, and the synthetic process includes processes such as esterification, acyl chloride, addition, reduction, chlorination, cyclization, hydrolysis and acidification. Among them, the addition reaction is 6-chloro-6-oxohexanoic acid ethyl ester obtained by esterification and acyl chloride of adipic acid, and ethylene addition reaction to prepare 6-oxo-8-chlorooctanoic aci...

Claims

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Application Information

Patent Timeline
17 Oct 2012
Publication
CN102731307A
IPC
C07C69/716; C07C67/347
Inventors
邹振荣; 钱振青