{[2-(2-Chloro-6-nitro-phenyl)-ethyl]-methyl-amino}-acetic Acid Ethyl Ester → {[2-(2-chloro-6-nitro-phenyl)-ethyl]-methyl-amino}-acetic Acid
反応式
C([O:3][C:4](=[O:20])[CH2:5][N:6]([CH2:8][CH2:9][C:10]1[C:15]([N+:16]([O-:18])=[O:17])=[CH:14][CH:13]=[CH:12][C:11]=1[Cl:19])[CH3:7])C>Br.C(#N)C>[Cl:19][C:11]1[CH:12]=[CH:13][CH:14]=[C:15]([N+:16]([O-:18])=[O:17])[C:10]=1[CH2:9][CH2:8][N:6]([CH2:5][C:4]([OH:20])=[O:3])[CH3:7]参加物
4
反応条件
- 温度
- 70 °C
実験手順
{[2-(2-chloro-6-nitro-phenyl)-ethyl]-methyl-amino}-acetic acid ethyl ester (11.0 g, 0.0365 mole) dissolved in concentrated hydrobromic acid (48 wt. % in water, 200 mL) was allowed to stir at 70° C. overnight and then reduced to a small volume in vacuo. The residue oil was taken up in acetonitrile and the solution was evaporated in vacuo. This procedure was repeated until the water was removed and a crystalline residue remained. This material was used in the next step without further purification.