Reacción #2936

Ecuación de reacción

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

tetra-n-butylammonium fluoride

→

title compound

Rendimiento 94.7%

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

Rendimiento 94.7%

Disolventes

tetrahydrofuran

tetrahydrofuran

Condiciones de reacción

Tratamiento posterior

1. 1
   OtroAfter removal of the cooling bath, it
2. 2
   workup.STIRRINGwas stirred further for 2 hours
3. 3
   workup.ADDITIONWater and n-hexane were added to the reaction solution
4. 4
   Otroafter vigorous shaking, the aqueous layer was separated out
5. 5
   LavadoThe aqueous layer was washed with chloroform three times

Procedimiento

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)

Fuente