{[2-(4-Chloro-2-nitro-phenyl)-ethyl]-methyl-amino}-acetic Acid Ethyl Ester → {[2-(4-chloro-2-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[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][C:11]=1[N+:17]([O-:19])=[O:18])[CH3:7])C>Br.C(#N)C>[Cl:16][C:13]1[CH:14]=[CH:15][C:10]([CH2:9][CH2:8][N:6]([CH2:5][C:4]([OH:20])=[O:3])[CH3:7])=[C:11]([N+:17]([O-:19])=[O:18])[CH:12]=1参加物
4
反応条件
- 温度
- 70 °C
実験手順
{[2-(4-Chloro-2-nitro-phenyl)-ethyl]-methyl-amino}-acetic acid ethyl ester (22.5 g, 0.075 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 (18.5 g) was used in the next step without further purification.