HRID2840

反应详情

EQUATION

反应方程式

HRID 2840 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-30 °C

PROCEDURE

实验过程

A solution of 1.38 g of the tris(2,4-bis(N,N-bis(2-t-butyldimethylsilyloxyethyl)sulfamoyl)phenyl)bismuthine preparation obtained in Example 5 in 15 ml of tetrahydrofuran was cooled to -30° C., and 5.88 ml of a 1 M/1 tetrahydrofuran solution of tetra-n-butylammonium fluoride was gradually added droprise under stirring. After removal of the cooling bath, it was stirred further for 2 hours. Water and n-hexane were added to the reaction solution, and after vigorous shaking, the aqueous layer was separated out. The aqueous layer was washed with chloroform three times, and lyophilized. As a result, 0.67 g of the title compound as obtained. NMR (D2O)δ: 8.49 (3H,s), 7.38, 6.82 (each 3H,A Bq), 3.65 (24H,m), 3.44 (12H,t), 3.29(12H,t)

WORKUP

后处理

  1. customAfter removal of the cooling bath, it
  2. stirringwas stirred further for 2 hours
  3. additionWater and n-hexane were added to the reaction solution
  4. customafter vigorous shaking, the aqueous layer was separated out
  5. washThe aqueous layer was washed with chloroform three times