HRID745606

反应详情

EQUATION

反应方程式

HRID 745606 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.93 g of triethylamine are added to the suspension of 0.7 g of 3,3-dimethylindoline-2-carboxylic acid hydrochloride in 20 ml of methylene chloride and the resulting solution is cooled to -10°. The solution of 0.51 g of 3-acetylthiopropanoyl chloride in 5 ml of methylene chloride is added dropwise and the mixture stirred at -5° to -10° for 1 hour and at room temperature for 3 hours. It is cooled to 0° and treated with 10 ml of 3N hydrochloric acid. The organic layer is separated and the aqueous solution further extracted with methylene chloride. The combined methylene chloride solutions are dried and evaporated, to give the 1-(3-acetylthiopropanoyl)-3,3-dimethylindoline-2-carboxylic acid as a foam.

WORKUP

后处理

  1. temperaturethe resulting solution is cooled to -10°
  2. temperatureIt is cooled to 0°
  3. customThe organic layer is separated
  4. extractionthe aqueous solution further extracted with methylene chloride
  5. dry with materialThe combined methylene chloride solutions are dried
  6. customevaporated