Preparation method of cyclopropyl acetylene important intermediate cyclopropylmethyl ketone

Abstract

The invention relates to a preparation method of a cyclopropyl acetylene important intermediate cyclopropylmethyl ketone. The invention adopts a technical scheme that: 5-chloro-2-pentanone is adopted as an initial raw material; under an alkaline condition and in a multistage reactor, a reaction is carried out with a reactive distillation technology, wherein a reaction temperature is controlled at 90-150 DEG C; and cyclopropylmethyl ketone is obtained in the multistage reactor. According to the invention, the reaction is carried out with the reactive distillation technology. Reaction and distillation are carried out simultaneously, such that the reaction process is simplified. Therefore, the operation is simple, and reaction can be continuously carried out. A cyclization reaction is carried out in the multistage reactor, such that space-time yield and selectivity of the reaction are improved. The reaction is carried out with the reactive distillation technology, such that reaction product is continuously removed, and reaction conversion rate is greatly improved. Because reaction selectivity and conversion rate are improved, three-waste production is greatly reduced, original steps of stratification and extraction are eliminated, and cost is reduced. The method is a green synthesizing process.

Description

technical field [0001] The invention relates to a preparation method of cyclopropylmethyl ketone, an important intermediate of cyclopropyne. Background technique [0002] Cyclopropyl methyl ketone, the English name of Cyclopropyl methyl ketone, is a yellow or slightly yellow transparent liquid with a certain solubility in water and can be miscible with alcohol ethers. The molecular formula is as follows [0003] . [0004] [0005] Cyclopropyl methyl ketone is an important intermediate in the synthesis of cyclopropyne, which is an important intermediate in the anti-AIDS drug efavirenz. Cyclopropylmethyl ketone is an indispensable drug intermediate for the synthesis of such drugs, and is of great significance for the synthesis of cyclopropyne. [0006] Synthetic methods of cyclopropyl methyl ketone are generally divided into the following categories: [0007] 1. CN1994996 reports a preparation method of cyclopropyl methyl ketone. Add acetyl n-propanol to hydrochloric ...

AI Technical Summary

Problems solved by technology

[0010] In addition, there are synthetic methods using cyclopropylethanol as raw materials and synthetic methods using cyclopropylnitroethane as raw materials, which are expensive and have no industrial value.

[0011] In summary, there are various defects in the existing synthetic methods, or the yield is low, or the raw materials are not easy to obtain, or the raw materials used are too dangerous to be conducive to industrial production, or the cost of raw materials is relatively expensive, or Is the operation process is cumbersome, poor product quality and other defects

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