反应详情

温度

60 °C

Lithium aluminum hydride (150 mg, 4.10 mmol) was suspended in tetrahydrofuran (5 mL), and the suspension was mixed with a solution of tert-butyl 4-morpholin-2-ylmethylpiperazinecarboxylate (390 mg, 1.37 mmol) prepared as an intermediate according to Process Step 2 of Reference Example 19 in tetrahydrofuran (5 mL) added dropwise under ice-cooling, followed by heating at 60° C. under reflux for two hours. An aqueous sodium hydroxide solution (2 mol/L, 10 mL) and chloroform (50 mL) were added under ice-cooling, followed by separation. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure, to thereby yield the title compound (180 mg, in a yield of 66%).

1. customprepared as an intermediate
2. additionadded dropwise under ice-
3. temperaturecooling
4. temperatureunder reflux for two hours
5. temperaturecooling
6. customfollowed by separation
7. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
8. distillationthe solvent was distilled off under reduced pressure