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Preparation method of ethyl 2-chloropropionate

A technology of ethyl chloropropionate and chloropropionyl chloride, applied in the chemical industry, can solve problems such as increasing environmental protection pressure and restricting the development prospects of products

Inactive Publication Date: 2018-01-05
李昊淼
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Defects and deficiencies of the prior art: the traditional process takes lactic acid, ethanol, thionyl chloride as main raw materials, and through esterification and chlorination two-step reaction, synthesizes high-purity ethyl 2-chloropropionate
However, this process requires the recovery of solvent benzene and the treatment of reaction wastewater, which increases the pressure on environmental protection and restricts the development of the product.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0017] A preparation method of ethyl 2-chloropropionate is to use 2-chloropropionyl chloride and ethanol in a molar ratio of 1:1 to 3, and carry out an alcoholysis reaction for 20 to 60 minutes at 10 to 20°C under anhydrous conditions, The ethyl 2-chloropropionate was obtained.

[0018] The ethanol mass concentration is 99%.

[0019] The preparation method of ethyl 2-chloropropionate comprises steps:

[0020] 1) Add 1 part by weight of 2-chloropropionyl chloride to the reaction vessel, heat in a water bath, keep the temperature at 10-20°C, and add 1-3 parts by weight of ethanol with a mass concentration of 99% dropwise with a dropping funnel;

[0021] 2) After the dropwise addition, quickly raise the temperature to 75°C to drive away the HCl remaining in the system. When the tail gas is absorbed and no more bubbles are generated, use an oil bath to heat, carry out vacuum distillation, and collect 30-50°C The low boiling fraction is returned to the jacket for use;

[0022] 3...

Embodiment 1

[0028] A preparation method of ethyl 2-chloropropionate is to use 2-chloropropionyl chloride and ethanol in a molar ratio of 1:1, and carry out an alcoholysis reaction for 50 to 60 minutes at 10°C under anhydrous conditions to obtain the described Ethyl 2-chloropropionate.

[0029] The ethanol mass concentration is 99%.

[0030] The preparation method of ethyl 2-chloropropionate comprises steps:

[0031] 1) Add 1 part by weight of 2-chloropropionyl chloride to the reaction vessel, heat in a water bath, keep the temperature at 10°C, and add 1 part by weight of ethanol with a mass concentration of 99% dropwise with a dropping funnel;

[0032] 2) After the dropwise addition, quickly raise the temperature to 75°C to drive away the HCl remaining in the system. When the tail gas is absorbed and no more bubbles are generated, use an oil bath to heat, carry out vacuum distillation, and collect low-boiling liquid at 30°C. Fraction back to use;

[0033] 3) start to collect the finish...

Embodiment 2

[0039] A preparation method of ethyl 2-chloropropionate is to use 2-chloropropionyl chloride and ethanol in a molar ratio of 1:2, and carry out alcoholysis reaction for 35-50 minutes at 15°C under anhydrous conditions to obtain the described Ethyl 2-chloropropionate.

[0040] The ethanol mass concentration is 99%.

[0041] The preparation method of ethyl 2-chloropropionate comprises steps:

[0042] 1) Add 1 part by weight of 2-chloropropionyl chloride to the reaction vessel, heat in a water bath, keep the temperature at 15°C, and add 2 parts by weight of ethanol with a mass concentration of 99% dropwise with a dropping funnel;

[0043] 2) After the dropwise addition, quickly raise the temperature to 75°C to drive away the HCl remaining in the system. When the tail gas is absorbed and no more bubbles are generated, use an oil bath to heat, carry out vacuum distillation, and collect low-boiling liquid at 35°C. Fraction back to use;

[0044] 3) start to collect the finished pr...

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PUM

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Abstract

The invention discloses a preparation method of ethyl 2-chloropropionate. According to the preparation method, 2-chloropropionyl chloride and ethanol undergo an alcoholysis reaction at the molar ratioof 1: 1-3 at 5-20 DEG C under the anhydrous condition for 20-60 min, so as to prepare the ethyl 2-chloropropionate. The new process is conducted under the anhydrous condition. No sewage is generatedduring the process, and there is no environmental protection pressure.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a preparation method of ethyl 2-chloropropionate. Background technique [0002] Ethyl 2-chloropropionate is a slightly aromatic, irritating, colorless, transparent liquid. Ethyl 2-chloropropionate is an important intermediate of α-substituted propionic acid series herbicides, plant growth regulators, and non-steroidal anti-inflammatory, antipyretic and analgesic drugs, such as dipropen, fluazifop, etc. It is widely used in the synthesis of herbicides, etc., and can also be used as an intermediate for spices and synthetic spices, such as raw materials for the synthesis of furanone. [0003] Defects and deficiencies of the prior art: the traditional process takes lactic acid, ethanol, and thionyl chloride as main raw materials, and through esterification and chlorination two-step reaction, synthesizes high-purity ethyl 2-chloropropionate. However, this process requires ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/14C07C69/63
Inventor 李昊淼
Owner 李昊淼
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