HRID131534
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 60 °C
PROCEDURE
实验过程
5.00 g tetrahydrothiopyran-4-one were dissolved in 15 ml acetonitrile, and 4.03 g N,N-dimethyl-methylenammonium chloride, followed by 40 μl acetyl chloride, were added. After the mixture had been stirred at a bath temperature of 60° C. for 45 minutes, it was stirred at room temperature for 60 hours and the precipitate formed was filtered off with suction and dried. 8.17 g 3-dimethylaminomethyl-tetrahydrothiopyran-4-one hydrochloride with a melting point of 155-157° C. were obtained. The corresponding base was liberated from this with methylene chloride and sodium hydroxide solution (32 percent strength by weight).
WORKUP
后处理
- additionwere added
- stirringit was stirred at room temperature for 60 hours
- customthe precipitate formed
- filtrationwas filtered off with suction
- customdried