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Preparation method of 4-chlorobenzhydrol

A technology of chlorobenzhydryl alcohol and chlorobenzophenone, which is applied in the field of preparation of 4-chlorobenzhydryl alcohol, can solve the problems of low yield of 4-chlorobenzhydryl alcohol, complex process, large energy consumption, etc. Simple, low energy consumption, low pollution effect

Inactive Publication Date: 2017-02-15
枣阳凤泽环化科技有限公司
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Problems solved by technology

[0006] The purpose of the present invention is to overcome the deficiencies in the prior art, to provide a kind of preparation method of 4-chlorobenzhydryl alcohol, to solve the problem of low yield, complicated process, large pollution and energy loss in the preparation of existing 4-chlorobenzhydryl alcohol costly technical issues

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Embodiment Construction

[0014] In order to better understand the present invention, the present invention will be described in detail below in conjunction with specific examples.

[0015] Using methanol, water, sodium hydroxide, 4-chlorobenzophenone and aluminum powder as raw materials, and the ratio of the 4-chlorobenzophenone, aluminum powder, sodium hydroxide, methanol and water is 1mol:0.8 mol:1.3mol:850ml:150ml. The specific preparation method is as follows:

[0016] The first step S1: add methanol and water to the reaction kettle, keep the temperature at 15°C, add sodium hydroxide, and dissolve completely. Put 4-chlorobenzophenone into the reactor. After the 4-chlorobenzophenone is added, stir well, cool down to 40-45°C and keep warm for 5 minutes. Under the condition that the above-mentioned temperature of 40-45°C remains unchanged, put aluminum powder into the reaction kettle in batches and intervals. The weight of the aluminum powder dropped each time decreases, and the time interval bet...

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Abstract

The invention provides a preparation method of 4-chlorobenzhydrol. Methanol, water, sodium hydroxide, 4-chlorobenzophenone and aluminum powder are adopted as the raw materials, and the 4-chlorobenzophenon, aluminum powder, sodium hydroxide, methanol and water are in a ratio of 1mol:0.8mol:1.3mol:850ml:150ml. The preparation method includes: mixing methanol with water, adding sodium hydroxide and dissolving it completely; adding 4-chlorobenzophenone, stirring the substances fully and evenly, then raising the temperature of the reaction solution to 40-45DEG C; adding a small amount of aluminum powder in batches, and controlling the temperature of the reaction solution at 40-45DEG C; then further performing stirring at 40-45DEG C till a reaction endpoint; and conducting filtering while the reaction product is hot to obtain a 4-chlorobenzophenone crystal, and performing drying. The residue and alkaline water left by the preparation method of 4-chlorobenzhydrol are subjected to neutralization treatment, and the pollution to the environment is little. The preparation method of 4-chlorobenzhydrol provided by the invention has the advantages of simple process, high yield and low energy consumption.

Description

technical field [0001] The invention relates to a preparation method of 4-chlorobenzhydryl alcohol. Background technique [0002] 4-chlorobenzhydryl alcohol can be used as an important pharmaceutical intermediate. Now commonly used catalytic hydrogenation method, zinc powder reduction method or NaBH 4 Reduction method to produce 4-chlorobenzhydryl alcohol. However, the above three methods all have disadvantages, as follows: [0003] (1) A large amount of by-products will be reduced at the same time by catalytic hydrogenation, and the procedure for subsequent treatment of by-products is complicated; [0004] (2), when using the zinc powder reduction method, it is necessary to make the crude product earlier, and then react the crude product with sherwood oil, water, vitriol oil and gac to produce 4-chlorobenzhydryl alcohol; not only the process is complicated, Moreover, concentrated sulfuric acid has great pollution and damage to the environment and reaction equipment; ...

Claims

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Application Information

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IPC IPC(8): C07C29/143C07C33/46
CPCC07C29/143C07C33/46
Inventor 陈金勇
Owner 枣阳凤泽环化科技有限公司
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