反应详情

温度

70 °C

K2CO3 (12.4 g, 90.0 mmol), KI (8.29 g, 51.0 mmol) and morpholine (3.9 mL, 45.0 mmol) were added to a solution of (2R,5R)-4-benzyl-5-chloromethyl-2-methyl-piperazine-1-carboxylic acid tert-butyl ester (10.0 g, 30.0 mmol) in acetonitrile (150 mL). The reaction was stirred at 70° C. for 18 h. The solids were filtered off and the solvent was removed in vacuo. The residue was partitioned between DCM (150 mL) and water (150 mL). The organic phase was dried (MgSO4) and evaporated. Chromatography (SiO2, eluted with petrol-EtOAc 0-50%) gave the title compound (9.0 g, 77%) as a white solid. MS: [M+H]+=390.

1. filtrationThe solids were filtered off
2. customthe solvent was removed in vacuo
3. customThe residue was partitioned between DCM (150 mL) and water (150 mL)
4. dry with materialThe organic phase was dried (MgSO4)
5. customevaporated
6. washChromatography (SiO2, eluted with petrol-EtOAc 0-50%)