HRID1063911

反应详情

EQUATION

反应方程式

HRID 1063911 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of tert-butyl 2-[(S)-7-(5-bromo-2-thienyl)-1,1-dioxoperhydro-1,4-thiazepin-7-yl]acetate•(1R)-10 -camphorsulfonate (2.00 g), dimethylaminosulfonyl chloride (569 mg) and 2M aqueous sodium carbonate (10.6 ml) in dioxane (40 ml) was stirred for 2.5 days at room temperature. After the reaction solution was concentrated in vacuo, the mixture was diluted with water. The obtained suspension was stirred for 30 minutes under ice-cooling. The resulting solid was collected, washed with water and dried in vacuo to give tert-butyl 2-[(S)-7-(5-bromo-2-thienyl)-4-dimethylaminosulfonyl-1,1-dioxoperhydro-1,4-thiazepin-7-yl]acetate (1.449 g) as a white solid.

WORKUP

后处理

  1. concentrationAfter the reaction solution was concentrated in vacuo
  2. additionthe mixture was diluted with water
  3. stirringThe obtained suspension was stirred for 30 minutes under ice-
  4. temperaturecooling
  5. customThe resulting solid was collected
  6. washwashed with water
  7. customdried in vacuo