反应 #4835

反应方程式

propine

2-iodophenylsulfonamide

P(C6H5)3

→

phenylsulfonamide

溶剂

dimethylformamide

triethylamine

反应条件

后处理

1. 1
   其他is completely reacted
2. 2
   过滤The reaction mixture is filtered
3. 3
   浓缩the residue is concentrated in vacuo
4. 4
   其他The precipitate is isolated
5. 5
   其他dried
6. 6
   其他Recrystallisation from ethyl acetate/hexane

实验过程

To a solution of 28.3 g (0.1 mole) of 2-iodophenylsulfonamide in 350 ml of dimethylformamide and 100 ml of triethylamine are added 1.0 g of palladium dichloro-bis(triphenylphosphite) complex, PdCl2 [P(C6H5)3 ]2, and 0.5 g of copper(I) iodide (CuI). Gaseous propine is then introduced into this solution until the starting material is completely reacted. The reaction mixture is filtered and the residue is concentrated in vacuo and then taken up in water. The precipitate is isolated and dried. Recrystallisation from ethyl acetate/hexane yields 15.6 g (80%) of 2-propyn-1-yl)phenylsulfonamide with a melting point of 147°-149° C.

来源