反应 #2935

反应方程式

tris(2,4-bis(N,N-bis(2-t-butyldimethylsilyloxyethyl)sulfamoyl)phenyl)bismuthine

ethanol

p-toluenesulfonic acid monohydrate

→

title compound

收率 79.5%

Tris(2,4-bis(N,N-bis(2-hydroxyethyl)sulfamoyl)phenyl)bismuthine

收率 79.5%

溶剂

dichloromethane

反应条件

后处理

1. 1
   其他prepared in Example 5
2. 2
   workup.DISSOLUTIONwas dissolved in a mixed solvent
3. 3
   workup.ADDITIONwas added
4. 4
   温度The mixture was refluxed
5. 5
   温度cooled to room temperature
6. 6
   过滤The crystals were collected by filtration
7. 7
   洗涤washed with 29.5 ml of dichloromethane
8. 8
   其他dried

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.

来源