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A kind of preparation method of diphenylacetonitrile

A technology of diphenylacetonitrile and mandelonitrile, which is applied in the field of organic chemical synthesis, can solve the problems of low utilization rate of bromine, unfavorable health of front-line workers, strong lachrymatory effect, etc., and achieve the effect of reducing costs

Active Publication Date: 2016-06-15
常州市正锋光电新材料有限公司
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Problems solved by technology

[0005] The technical problem to be solved by the present invention is: in the prior art, in the process of preparing diphenylacetonitrile, bromine bromination and condensation of diphenylacetonitrile are used, the utilization rate of bromine is very low, and the intermediate product α-bromine Phenylacetonitrile has a strong tear gas effect, which is not conducive to the health of front-line workers

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  • A kind of preparation method of diphenylacetonitrile

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Embodiment Construction

[0014] (1) Add 133g of mandelonitrile and 600g of benzene into a four-necked flask equipped with a stirrer, condenser and thermometer, and add 50g of concentrated sulfuric acid with a solute mass fraction of 98% dropwise at 40-45°C for half an hour After the dropwise addition is completed, the reaction is stirred at 40-45°C for 1 hour until the reaction of mandelonitrile is complete;

[0015] (2) Pour the reaction system obtained in step (1) into 800 g of water, separate layers, remove the water layer, wash the organic layer with water, dry, recover benzene by atmospheric distillation, and distill the product under reduced pressure.

[0016] 150.5 g of diphenylacetonitrile was obtained, with a content of 99.2%, and a yield of 78% (calculated based on the conversion rate of mandelonitrile).

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Abstract

The invention belongs to the synthetic field of organic chemistry, and is particularly relates to a method for synthesizing diphenylacetonitrile by using mandelonitrile. The method comprises the steps of adding mandelonitrile and benzene into a reactor with a stirrer, a condenser and a thermometer; dropwise adding concentrated sulfuric acid at a temperature lower than 45 DEG C; reacting for 1 hour after concentrated sulfuric acid is completely added; adding water; layering; washing the oil layer with water; drying and distilling out benzene; and distilling out a product at a reduced pressure. The method synthesizes diphenylacetonitrile by using mandelonitrile, thereby preventing strong tearing property of alpha-bromobenzyl cyanide which is an intermediate prepared by using bromine. Besides, the method takes use of concentrated sulfuric acid as a condensing agent, thereby reducing cost.

Description

technical field [0001] The invention belongs to the field of organic chemical synthesis, in particular to a method for synthesizing diphenylacetonitrile by using mandelonitrile. Background technique [0002] Diphenylacetonitrile is a white crystal, soluble in ethanol and ether, but insoluble in water. Its use is mainly used as an intermediate in organic synthesis, and used in medicine to produce gastric amine; [0003] Diphenylacetonitrile on the market today is mainly obtained from bromine bromination and condensation of phenylacetonitrile. This brings about a series of problems: First, bromine is an unstable raw material: it evaporates quickly at room temperature, its vapor has a strong suffocating pungent smell, and is slightly soluble in water. Due to the volatility of bromine, when it is used as a raw material in industrial production, the utilization rate is too low. Under normal circumstances, the actual use of bromine in industry is often more than 1.2 times the th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/33C07C253/30
Inventor 徐小虎
Owner 常州市正锋光电新材料有限公司
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