反应详情

1-(Phenylmethyl)4-piperidinamine (3 g) in dichloromethane (10 mL) and triethylamine (4.5 mL) were added dropwise to a stirred solution of triphosgene (1.55 g) in dichloromethane (20 mL) at 0° C. under nitrogen. The reaction mixture was allowed to warm to room temperature and stirred for 30 minutes. The mixture was cooled to 0° C. and formyl hydrazine (1.4 g) and triethylamine (4.5 mL) were added. The reaction was stirred at room temperature for 1 hour and then evaporated to dryness. Purification (SiO2, methanol:dichloromethane:ammonium hydroxide solution 5:95:1 as eluant) gave the sub-title compound (2.5 g).

1. temperatureThe mixture was cooled to 0° C.
2. stirringThe reaction was stirred at room temperature for 1 hour
3. customevaporated to dryness
4. customPurification (SiO2, methanol:dichloromethane:ammonium hydroxide solution 5:95:1 as eluant)