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Citation: Tan Chunbin, Liu Xiaoling, Fang Aiquan, Du Hongfei. The Process Optimization on Synthesis of 3-Keto-4-carbomethoxythiophane[J]. Chemistry, ;2018, 81(10): 957-959. shu

The Process Optimization on Synthesis of 3-Keto-4-carbomethoxythiophane

Chongqing Academy of Chinese Materia Medica, Chongqing 400065

Corresponding author: Du Hongfei, t0913023@163.com
Received Date: 28 May 2018
Accepted Date: 26 June 2018

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3-Keto-4-carbomethoxythiophane (Ⅲ) was synthesized by Dieckmann cyclization reaction, using methanol and mercapto acetic acid as the starting materials. The structure of the product was confirmed by ¹H NMR, ¹³C NMR and HRMS. Effects of different organic or inorganic base types, reaction solvent and temperature on the cyclization reaction were investigated as well. The results showed that organic bases are superior to inorganic bases; high temperature is beneficial to give Ⅲ. The optimized process for the synthesis of compound Ⅲ is as follows:pyridine as base, toluene as solvent, react at 80℃ for 2 h. The yield of 3-Keto-4-carbomethoxythiophane reached 78%.
- 3-Keto-4-carbomethoxythiophane,
- Methyl acrylate,
- Methyl mercapto acetate,
- Process optimization
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