Synthesis process of cyclopentyl phenyl ketone

Abstract

The invention discloses a synthesis process of cyclopentyl phenyl ketone, and the synthesis process comprises the following steps: (1) adding excess 40g-4kg of magnesium chips into dried 120ml-12L of tetrahydrofuran, dropwise adding 30g-3kg of Bromocyclopentane, heating the Bromocyclopentane material as a base material to initiate reaction; (2) dropwise adding 700ml-70L of the tetrahydrofuran and the Bromocyclopentane into the reaction system, after completion of the adding of the tetrahydrofuran and the Bromocyclopentane, dropwise adding 107g-10kg of cyanobenzene, keeping temperature at 48-50 DEG C, after completion of the adding of the cyanobenzene, keeping the temperature for 2-3h, applying points for gas phase detection until 5% of the cyanobenzene is left; (3) using hydrochloric acid for quenching the reaction, after the reaction is quenched, regulating pH value to 4-5; and standing for layering to separate upper layer organic phase for rotary evaporation to dry; and (4) dropwise adding 3 times of the amount of methyl tertiary butyl ether into the rotary-evaporation-dried organic phase to precipitate a large amount of solid, filtering rotary-evaporation-dried filtrate, and distilling the rotary-evaporation-dried filtrate to obtain 51g-5kg of the product cyclopentyl phenyl ketone which is a light yellow liquid with a purity of more than 99%. The synthesis process has the advantages of less by-products and lower cost, can be used as a new synthetic process of medicines, has the advantages of simple operation, easy control, easy industrialization and high product purity, and solves the problem of low content.

Description

technical field [0001] The invention relates to a synthesis process of cyclopentyl phenyl ketone. Background technique [0002] Ketamine hydrochloride is a new fast and short-acting anesthetic of non-barbiturate separation, and it has been widely used in clinical practice now. Cyclopentyl phenyl ketone is an important intermediate for the synthesis of ketamine. [0003] Currently, Grignard reagent or organic zinc is used to synthesize phenylcyclopentyl ketone, which requires anhydrous and oxygen-free operation at a low temperature of -78°C or -45°C, which not only requires high energy consumption at low temperature, but also requires harsh operating conditions, which is not suitable for large-scale industrialization. Production. [0004] Therefore, it is necessary to provide a new technical solution to solve the above problems. Contents of the invention [0005] The technical problem to be solved by the present invention is to provide a synthesis process of cyclopentyl p...

AI Technical Summary

Problems solved by technology

[0003] Currently, Grignard reagent or organic zinc is used to synthesize phenylcyclopentyl ketone, which requires anhydrous and oxygen-free operation at a low temperature of -78°C or -45°C, which not only requires high energy consumption at low temperature, but also requires harsh operating conditions, which is not suitable for large-scale industrialization. Production