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A kind of preparation method of cyclopropylamine intermediate methyl cyclopropanate

A technology of methyl cyclopropanate and intermediates, which is applied in the field of preparation of cyclopropylamine intermediate methyl cyclopropanate, which can solve the problems of incomplete reaction, difficult to control yield, high impurity content of products, etc., so as to avoid environmental pressure , Reduce the cost of raw materials, the effect of high product yield

Active Publication Date: 2020-08-18
SHANDONG GUOBANG PHARMA
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Problems solved by technology

The industrial sodium methoxide is a low-concentration methanol solution, so the methanol needs to be distilled during the cyclization reaction. The sodium methoxide precipitated during the treatment is easy to adhere to the side wall of the reactor, resulting in incomplete reaction and difficult to control the yield. The impurity content in the product is more; And when adopting sodium methoxide to handle methyl cyclopropanate, a large amount of methanol will circulate in the system, which will affect the cooling and heating of the reaction, resulting in large power consumption and production The cost increases; there is also the sodium methylate that is cyclized to γ-chlorobutyric acid methyl ester is synthesized by sodium method or alkali method, and this synthesis has a higher raw material cost

Method used

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  • A kind of preparation method of cyclopropylamine intermediate methyl cyclopropanate

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Embodiment 1

[0020] In a 1000ml reactor, add 1 mol of calcium carbide, seal it and replace the air with nitrogen for 3 times, then start to add 4 mol of methanol dropwise, and collect acetylene gas until the reaction is completed. Then add 1.8mol of methyl γ-chlorobutyrate dropwise to the reactor, control the drop rate and keep the temperature constant at 100°C, and collect the methanol fraction generated during the dropwise addition process. After the reaction is over, collect the fraction by heating up and distilling , 170.3 g of methyl cyclopropanecarboxylate was obtained, and the yield was 94.5%.

Embodiment 2

[0022] In a 1000ml reactor, add 1 mol of calcium carbide, seal it and replace the air with nitrogen for 3 times, then start to add 2 mol of methanol dropwise, and collect acetylene gas until the reaction is completed. Then add 1.8mol of methyl γ-chlorobutyrate dropwise to the reactor, control the drop rate and keep the temperature constant at 100°C, and collect the methanol fraction generated during the dropwise addition process. After the reaction is over, collect the fraction by heating up and distilling , 150.1 g of methyl cyclopropanate was obtained, with a yield of 83.3%.

Embodiment 3

[0024] In a 1000ml reactor, add 1mol of calcium carbide, seal it and replace the air with nitrogen for 3 times, then start to add 6mol of methanol dropwise, and collect acetylene gas until the reaction is completed. Then add 1.8mol of methyl γ-chlorobutyrate dropwise to the reactor, control the drop rate and keep the temperature constant at 100°C, and collect the methanol fraction generated during the dropwise addition process. After the reaction is over, collect the fraction by heating up and distilling , 120.5 g of methyl cyclopropanate was obtained, with a yield of 66.9%.

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Abstract

The invention discloses a method for preparing cyclopropylamine midbody cyclopropanecarboxylic acid methyl ester. First in a sealed reaction kettle, methanol is added dropwise into calcium carbide, togenerate calcium methoxide and acetylene; gamma-chloro methyl butyrate is added into calcium methoxide at 60-120 DEG C, the temperature is controlled to be constant in the reaction process, methanolgenerated in the process is collected, and the cyclopropanecarboxylic acid methyl ester is obtained through distillation. The method is simple in process, types of raw materials necessary for production are fewer, some of the raw materials can be reused, the yield is high, the quality is good, and the method is safe and environmentally friendly.

Description

technical field [0001] The invention relates to the technical field of synthesis of pharmaceutical intermediates, in particular to a method for preparing a cyclopropylamine intermediate, methyl cyclopropanate. Background technique [0002] At present, there are many technological routes for producing methyl cyclopropanate, but the main production route is that methyl γ-chlorobutyrate is dehydrochlorinated by sodium methoxide to form a ring to generate methyl cyclopropanate. The industrial sodium methoxide is a low-concentration methanol solution, so the methanol needs to be distilled during the cyclization reaction. The sodium methoxide precipitated during the treatment is easily attached to the side wall of the reactor, resulting in incomplete reaction and difficult to control the yield. The impurity content in the product is more; And when adopting sodium methylate to process methyl cyclopropanate, a large amount of methanol will circulate in the system, which will affect ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/333C07C69/74
CPCC07C29/70C07C67/333C07C69/74C07C31/30
Inventor 陆华文李琦斌王伟宏廖仕学李进伟刘聪
Owner SHANDONG GUOBANG PHARMA
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