HRID21732

反应详情

EQUATION

反应方程式

HRID 21732 的结构方程式

PROCEDURE

实验过程

A solution of 1,4 g 2,4-dichloro-6-fluoro-7-[N-(2,2-dimethylpropanoyl)hydrazino]benzothiazole in 8 ml of a 20% solution of phosgene in toluene was heated for 8 hours at 100° C. After cooling, the toluene was removed in vacuo and the residue taken up in dichloromethane. The extract was shaken with aqueous sodium hydrogen carbonate and water, dried over magnesium sulfate and concentrated. The residue was recrystallised from isopropanol/diisopropyl ether. Yield: 0.5 g=40% of theory. m.p.: 157°-158° C.

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe toluene was removed in vacuo
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated
  5. customThe residue was recrystallised from isopropanol/diisopropyl ether