反应详情

Morpholin-3-one (896 mg, 8.87 mmol) was added to a slurry of NaH (60% in mineral oil, 355 mg, 8.87 mmol) in DMF (10 mL) under N2. The suspension was stirred for 30 minutes at room temperature and then a solution of (2R,5R)-4-benzyl-5-chloromethyl-2-methyl-piperazine-1-carboxylic acid tert-butyl ester (2.0 g, 5.9 mmol) in DMF (10 mL) was slowly added. The resulting mixture was stirred at 65° C. for 2 h. The reaction was cooled to room temperature and partitioned between EtOAc and saturated aqueous NaHCO3. The organic phase was dried over MgSO4 and concentrated in vacuo. Chromatography (50% EtOAc in petrol) gave the title compound (1.76 g) as a pale yellow gum. MS: [M+H]+=404.

1. stirringThe resulting mixture was stirred at 65° C. for 2 h
2. temperatureThe reaction was cooled to room temperature
3. custompartitioned between EtOAc and saturated aqueous NaHCO3
4. dry with materialThe organic phase was dried over MgSO4
5. concentrationconcentrated in vacuo