Method using micro reactor to prepare 1-chloro-1'-chloroacetyl cyclopropane

A chloroacetylcyclopropane, microreactor technology, applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve the problem of long reaction operation time, increase of "three wastes", poor reaction selectivity, etc. problems, to achieve the effect of mild conditions, environmental friendliness, and easy industrialization

Active Publication Date: 2016-03-09
大连科铎环境科技有限公司
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  • Abstract
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Problems solved by technology

[0003] The conventional method is to use sulfuryl chloride etc. as a chlorination reagent to carry out chlorination reaction on the α-position hydrogen atom of the substrate carbonyl group, but the reaction is exothermic violently, there are serious local overheating problems and heat tra

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  • Method using micro reactor to prepare 1-chloro-1'-chloroacetyl cyclopropane
  • Method using micro reactor to prepare 1-chloro-1'-chloroacetyl cyclopropane
  • Method using micro reactor to prepare 1-chloro-1'-chloroacetyl cyclopropane

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[0022] The application also provides a preparation method of 1-chloro-1'-chloroacetylcyclopropane, that is, using 1-chloro-1'-acetylcyclopropane and chlorine gas as raw materials to realize the chlorine of the α-position hydrogen atom in the microchannel A substitution reaction to generate 1-chloro-1'-chloroacetylcyclopropane can be carried out under solvent-free or solvent-free conditions. However, it is preferably carried out under solvent-free conditions. Specifically, the microreactor device is used to prepare the method for 1-chloro-1 '-chloroacetylcyclopropane, comprising the steps:

[0023] 1) Prepare the raw materials 1-chloro-1′-acetylcyclopropane and chlorine gas for later use;

[0024] 2) Feed the raw materials through different feed pumps according to a certain ratio, and react through the micro-reaction channel. The reaction time is 0.15-10min, the temperature is -20-100°C, and the pressure is 1-2atm;

[0025] 3) The flow state of the mixed liquid in step 2) is ...

Embodiment 1

[0027]

[0028] Adjust the temperature of the temperature control device to 10°C and the system pressure to 1 atm. Under the condition of no solvent, adjust the flow rate of the substrate to 10mol / h, the flow rate of chlorine gas to 10.5~11mol / h, and use a metering pump to inject the material into the reaction system. Reaction, according to the requirements of the reaction, the control reaction time is 30s. As the reaction progressed, the temperature at the outlet of the reactor gradually increased to 25°C, and the temperature at the outlet of line 2 increased to 20°C. After 2 hours of reaction, samples were taken for gas phase analysis. The GC normalized purity of the product was 99.2%, and the quantitative yield was 98.5%.

Embodiment 2

[0030]

[0031] Adjust the temperature of the temperature control device to 10°C, and the system pressure to 1 atm. Under the condition that the solvent is toluene, adjust the substrate flow rate to 1mol / h, the chlorine gas flow rate to 1.0~1.15mol / h, and use a metering pump to inject the material into the reaction system According to the requirements of the reaction, the reaction time is controlled to be 20s. As the reaction progressed, the temperature at the outlet of the reactor gradually increased to 30°C, and the temperature at the outlet of pipeline 2 increased to 20°C. After 1 hour of reaction, samples were taken for gas phase analysis. The GC normalized purity of the product was 97.6%, and the quantitative yield was 96%.

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Abstract

The invention discloses a method using a micro reactor to prepare 1-chloro-1'-chloroacetyl cyclopropane. The reactions can be carried out in the presence or absence of a solvent. According to the preparation method, 1-chloro-1'-acetyl cyclopropane and chlorine gas are pumped into a micro reaction channel to carry out reactions by a feed pump according to a certain ratio. The device comprises a raw material bottle, a feed pump, a pre-heating or pre-cooling pipe, a micro reactor, a time delay pipe, a temperature controlling device, a counterbalance valve, and a product receiver. A micro reactor, which can quickly mix the raw materials and has a good heat exchange effect, is used as the reaction device; so that 1-chloro-1'-acetyl cyclopropane and chlorine gas can carry out high selective(alpha-position hydrogen atom) chlorination reactions in a micro channel under high speed and efficient mixing to generate 1-chloro-1'-chloroacetyl cyclopropane. The provided method has the advantages of simple operation, mild conditions, high selectivity, and low energy consumption; compared with the conventional reactions, the using amount of solvent is reduced, and moreover, the method is environment-friendly and can be easily applied to industrialization.

Description

technical field [0001] The invention belongs to the technical field of fine chemical technology, relates to chemical synthesis technology, and uses chlorine gas as a raw material and 1-chloro-1'-acetylcyclopropane as a new chlorination reaction method as a substrate. Background technique [0002] 1-Chloro-1'-chloroacetyl cyclopropane is widely used in medicine, pesticide, industrial fungicide and other fields. [0003] The conventional method is to use sulfuryl chloride etc. as a chlorination reagent to carry out chlorination reaction on the α-position hydrogen atom of the substrate carbonyl group, but the reaction is exothermic violently, there are serious local overheating problems and heat transfer problems of the reaction system, resulting in reaction selection Poor performance, unsatisfactory yield; too long reaction operation time, low production capacity; and the generated sulfur dioxide and other gases greatly increased the amount of "three wastes". Contents of the...

Claims

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Application Information

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IPC IPC(8): C07C45/63C07C49/327
CPCC07C45/63C07C49/327
Inventor 王善强杨宪斌赵光春曹丽贤张宇王乃伟
Owner 大连科铎环境科技有限公司
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