[Cl:1][CH2:2][C:3](Cl)=[O:4].[Cl:6][C:7]([Cl:20])([Cl:19])[CH:8]([NH2:18])[NH:9][C:10](=[O:17])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C(N(CC)CC)C.O>CC(C)=O>[Cl:6][C:7]([Cl:19])([Cl:20])[CH:8]([NH:9][C:10](=[O:17])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[NH:18][C:3](=[O:4])[CH2:2][Cl:1]Chloroacetyl chloride (79g) in acetone (100 ml) was added dropwise to a solution of 1,1,1-trichloro-2-amino-2-(benzamido)ethane (170g) in acetone (500 ml) containing triethylamine (64.2g). The mixture was stirred for 2 hours. The reaction mixture was poured into water (750 ml). The solid was collected, washed with water and dried (195g). Recrystallisation from nitromethane (or dioxane) gave pure 1,1,1-trichloro-2-benzamido-2-(chloroacetamido)ethane (156g, m.p. 210°-213°)
Wird geladen…