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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). The filtrate is concentrated under vacuum to provide crude title compound (11.40 g, 88%) as a yellow, crystalline solid. A sample (2 g) is recrystallized from cyclohexane and then from toluene to provide the purified title compound (0.83 g) as a fine, white crystals: mp 80–81° C.

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)
7. concentrationThe filtrate is concentrated under vacuum
8. customto provide crude title compound (11.40 g, 88%) as a yellow, crystalline solid
9. customA sample (2 g) is recrystallized from cyclohexane
10. customfrom toluene to provide the
11. custompurified title compound (0.83 g) as a fine, white crystals