Novel method for synthesizing 3-oxetanone

A technology of oxetanone and compound, which is applied in the field of synthesizing 3-oxetanone, can solve the problems of few 3-oxetanone manufacturers, hindering the development of downstream products, and low reaction yield. Achieve the effects of easy purification, reduced reaction cost, and simple operation

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A technology of oxetanone and compound, which is applied in the field of synthesizing 3-oxetanone, can solve the problems of few 3-oxetanone manufacturers, hindering the development of downstream products, and low reaction yield. Achieve the effects of easy purification, reduced reaction cost, and simple operation

CN102329286AActive Publication Date: 2012-01-25TIANJIN QUANHECHENG TECH

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[0015] 1. Hydrolysis, ring closure reaction

[0016] 1,3-Dichloroacetone (50g) was dissolved in anhydrous methanol (350mL), and methanol solution of sodium methoxide (30g, 700mL) was slowly added dropwise at 0°C. After the addition was complete, it was stirred at room temperature for 30min. TCL tracked the end of the reaction, slowly added water (3.6g) dropwise to the reaction solution, and controlled the dropping temperature to be 0°C. After the dropwise addition was completed, the temperature was raised to reflux, and the reaction was carried out for 6 hours. The reaction solution was concentrated to a volume of (100 mL), extracted with ethyl acetate, and the organic phases were combined, washed with brine, dried over sodium sulfate, and concentrated and rectified product 2 (39.2 g), with a yield of 84%.

[0017] 1,3-Dichloroacetone (500g) was dissolved in anhydrous methanol (3.5L), and a methanol solution of sodium methoxide (300g, 7L) was slowly added dropwise at 0°C. Afte...

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Abstract

The invention discloses a novel method for synthesizing 3-oxetanone. 1,3-dichloroacetone is taken as an initial raw material, a key intermediate is obtained through hydrolysis and ring-closing one-pot reaction, the yield is over 80 percent, the 3-oxetanone is obtained through deprotection, the total yield is over 50 percent, and the route is shown in the specification. The method has the advantages that: the use of a dangerous chemical reagent is avoided, the reaction route is shortened, the reaction cost is reduced, the reaction yield is improved, the method is easy to operate, and the industrialized production can be realized.

Description

technical field [0001] The invention relates to a new method for synthesizing 3-oxetanone. Background technique [0002] 3-Oxetanone is an important biopharmaceutical intermediate, which can be widely used in the synthesis of various drugs. It has a small molecular weight and a unique structure, and can be derived from a variety of downstream products, so it has a wide range of uses. At present, the method for synthesizing 3-oxetanone has the following several methods, but these methods involve the use of dangerous goods, such as sodium hydride, butyllithium, azidemethane, etc.; the reaction route is long, and the reaction yield is low. Generally no more than 10%; disadvantages such as inconvenient amplification make the manufacturers of 3-oxetanone very few and expensive, seriously hindering the development of its downstream products and its further development in the field of biomedicine. [0003] Synthetic route 1: [0004] [0005] Synthetic route 2: [0006] ...

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Application Information

Patent Timeline

25 Jan 2012

Publication

CN102329286A

IPC: C07D305/10

Inventors: 宋艳民; 陈鹏飞