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Method for synthesizing methyl cyclopropanecarboxylate

A technology for the synthesis of methyl cyclopropanecarboxylate, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds. And the effect of low use, low risk and energy saving

Inactive Publication Date: 2020-05-19
山东普润药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Calcium methoxide has poor catalytic ability and low reaction yield; sodium methoxide and potassium methoxide are dangerous chemicals, flammable in contact with water, direct purchase has high requirements for storage and use, and the price is very expensive, which has a negative impact on the raw material cost of the product. It has a great impact; if it is self-made, it needs to use metal sodium or metal potassium. These two metals are more dangerous than sodium methoxide and potassium methoxide, and a large amount of hydrogen gas is produced during the reaction, so the risk of the reaction is extremely high
Mixed solvents of xylene and methanol will be produced after the reaction with the above catalysts is completed, which brings difficulties to solvent recovery and requires a large amount of energy consumption, and the recovery rate of methanol with general recovery equipment is very low, and the water requirement for recovery of methanol is very low. Very high, not suitable for industrial production

Method used

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  • Method for synthesizing methyl cyclopropanecarboxylate
  • Method for synthesizing methyl cyclopropanecarboxylate

Examples

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Embodiment 1

[0016] A method for synthesizing methyl cyclopropanate, adding 800-1200g of potassium carbonate to a clean 1800-2200ml reaction bottle, then adding 800-900g of xylene, and adding methyl chlorobutyrate 740 dropwise at a temperature of 85-100°C -920g, after dripping, control the temperature at 85-100°C for 1-5h, cool down to 30-50°C at the end of the heat preservation, filter, wash the filter cake with xylene, combine the filtrate, and rectify the filtrate to obtain methyl cyclopropanate 522 -602g, the yield is 90-98%, and xylene is recovered and applied mechanically.

Embodiment 2

[0018] In the synthetic method of methyl cyclopropanate described in Example 1, 1000 g of potassium carbonate was added in a clean 2000 ml reaction bottle, and then 860 g of xylene was added, and 780 g of methyl chlorobutyrate was added dropwise at a temperature of 85 to 100° C. After completion, control the temperature at 85-100°C for 3 hours, cool down to below 40°C at the end of the heat preservation, filter, wash the filter cake with xylene, combine the filtrate, and rectify the filtrate to obtain 562g of methyl cyclopropanate, with a yield of 95%. Recycling.

Embodiment 3

[0020] Synthetic method of methyl cyclopropanate described in embodiment 1, in clean 1800ml reaction bottle, add salt of wormwood 800g, then add dimethylbenzene 800g, control temperature and drop methyl chlorobutyrate 740g at 85 ℃, dripping finishes, Control the temperature at 85°C for 1 hour, cool down to below 30°C at the end of the heat preservation, filter, wash the filter cake with xylene, combine the filtrate, and rectify the filtrate to obtain 522g of methyl cyclopropanate, with a yield of 90%. The xylene is recovered and used mechanically.

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Abstract

The invention discloses a method for synthesizing methyl cyclopropanecarboxylate. The method comprises the following steps: adding 800-1200 g of potassium carbonate into a clean 1800-2200 ml reactionbottle; adding 800-900 g of xylene, controlling the temperature to be 85 to 100 DEG C, and adding 740-920 g of methyl chlorobutyrate in a dropwise manner; after dropping is finished, controlling the temperature to be 85-100 DEG C, and carrying out heat preservation for 1-5 h; and after heat preservation is finished, cooling is conducted to less than 30-50 DEG C, filtering, washing the filter cakewith xylene, combining the filtrate, and rectifying the filtrate to obtain 522-602 g of methyl cyclopropanecarboxylate, wherein the yield is 90-98%, and xylene is recycled and reused. The method is used for synthesizing methyl cyclopropanecarboxylate.

Description

technical field [0001] The invention relates to a method for synthesizing methyl cyclopropanate. Background technique [0002] Methyl cyclopropanate is an important pharmaceutical and pesticide intermediate. In industrial production, methyl chlorobutyrate is mainly used as a raw material, and sodium methylate, calcium methylate, and potassium methylate are used as catalysts to synthesize methyl cyclopropanate. [0003] Calcium methoxide has poor catalytic ability and low reaction yield; sodium methoxide and potassium methoxide are dangerous chemicals, flammable in contact with water, direct purchase has high requirements for storage and use, and the price is very expensive, which has a negative impact on the raw material cost of the product. It has a great impact; if it is self-made, metal sodium or metal potassium is needed. These two metals are more dangerous than sodium methoxide and potassium methoxide, and a large amount of hydrogen gas is produced during the reaction, ...

Claims

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Application Information

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IPC IPC(8): C07C67/333C07C69/74
CPCC07C67/333C07C69/74
Inventor 苑文秋舒茂胜蔡跃冬陈航军
Owner 山东普润药业有限公司
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