反応 #4835

反応方程式

propine

2-iodophenylsulfonamide

P(C6H5)3

→

phenylsulfonamide

溶媒

dimethylformamide

triethylamine

反応条件

後処理

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

実験手順

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.

出典