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温度

0 °C

To a suspension of 3-benzyl-piperazine-2,5-dione (14.98 g, 73 mmol, prepared following generally the procedure of Halpern and Westley, J. Org. Chem. 1968, 33, 864) in dry diethyl ether (500 mL) is added dropwise to a solution of lithium aluminum hydride (400 mL of a 1 M solution in diethyl ether, 400 mmol, 5.4 eq). The suspension is heated at reflux for 23 hours and then cooled to 0° C. Water (70 mL) is then cautiously added and the resulting suspension is warmed to room temperature. After 3 hours the suspension is filtered and the solid washed with diethyl ether (1 L).

1. customprepared
2. temperatureThe suspension is heated
3. temperatureat reflux for 23 hours
4. temperaturethe resulting suspension is warmed to room temperature
5. filtrationAfter 3 hours the suspension is filtered
6. washthe solid washed with diethyl ether (1 L)