1-Carbethoxy-4-(5-chloro-2-nitroanilino)-piperidine → Domperidone Impurity 12
反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N+:20]([O-])=O)=[C:6]([NH:8][CH:9]2[CH2:14][CH2:13][N:12]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:11][CH2:10]2)[CH:7]=1>CO.[Pt]>[NH2:20][C:5]1[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][C:6]=1[NH:8][CH:9]1[CH2:10][CH2:11][N:12]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:13][CH2:14]1参加物
4
実験手順
A suspension of D5 (15.0 g, 45 mmol) and 5% Pt/C (1.5 g) in methanol (500 mL) in an autoclave (1000 mL) was put under an atmosphere of hydrogen (˜40 atm). The mixture was stirred at room temperature for 3 hours and then filtered through a pad of celite. The filtrate was concentrated under reduced pressure to give the title compound (13.5 g, 100% yield) as a dark brown solid that was used without further purification. (Rf: 0.3 (ethyl acetate/hexane 7:8))