反应详情

1M Lithium aluminium hydride in tetrahydrofuran (112 ml, 0.112 mol) was added dropwise to a stirred solution of (RS)-1-benzyl-4-(tert-butyloxycarbonyl)-2-carbamoylpiperazine (D1) (15 g, 0.047 mol) in anhydrous tetrahydrofuran (300 ml) at room temperature under argon. On complete addition the reaction mixture was stirred at room temperature for 0.5 h, then at reflux for a further 1.5 h. The mixture was cooled to room temperature and treated sequentially with water (19.5 ml), 2N sodium hydroxide (22.5 ml) and water (19.5 ml) dropwise. Sodium sulphate was added and the resultant stirred for 0.3 h, filtered and the filtrate evaporated in vacuo to give the title compound (10.3 g, 100%).

1. additionOn complete addition the reaction mixture
2. temperatureat reflux for a further 1.5 h
3. temperatureThe mixture was cooled to room temperature
4. stirringthe resultant stirred for 0.3 h
5. filtrationfiltered
6. customthe filtrate evaporated in vacuo