HRID2839

反应详情

EQUATION

反应方程式

HRID 2839 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

13.59 g of the tris(2,4-bis(N,N-bis(2-t-butyldimethylsilyloxyethyl)sulfamoyl)phenyl)bismuthine preparation prepared in Example 5 was dissolved in a mixed solvent containing 13.6 ml of ethanol and 27 ml of dichloromethane, and 0.272 g of p-toluenesulfonic acid monohydrate was added thereto. The mixture was refluxed under heating at 50° C. for 6 hours, and then cooled to room temperature. The crystals were collected by filtration, washed with 29.5 ml of dichloromethane and dried. As a result, 5.54 g of the title compound was obtained as crystals with a melting point of 110°-113° C.

WORKUP

后处理

  1. customprepared in Example 5
  2. dissolutionwas dissolved in a mixed solvent
  3. additionwas added
  4. temperatureThe mixture was refluxed
  5. temperaturecooled to room temperature
  6. filtrationThe crystals were collected by filtration
  7. washwashed with 29.5 ml of dichloromethane
  8. customdried