反应详情

温度

60 °C

A suspension of 3-(2,3-dimethoxybenzyl)-2,5-piperazinedione (1.26 g) in a mixed solvent of tetrahydrofuran (50 ml) and 1,2-dimethoxyethane (50 ml) was heated at 60° C. with stirring and lithium aluminum hydride (0.905 g) was added thereto portionwise carefully. After the reaction mixture was heated at 70° C. with stirring for 3 hours, lithium aluminum hydride (0.20 g) and tetrahydrofuran (30 ml) were added thereto again and the suspension was stirred at the same temperature for 12 hours. After being cooled with ice-water, the mixture was quenched by sequential addition of water (1.3 ml), 15% aqueous sodium hydroxide (1.3 ml), water (3.8 ml) and the whole was stirred at room temperature for 2 hours. The resulting insoluble materials were removed by filtration and the filtrate was dried over sodium sulfate, and evaporated under reduced pressure to give light yellowish oil of 2-(2,3-dimethoxybenzyl)piperazine (0.97 g).

1. temperatureAfter the reaction mixture was heated at 70° C.
2. stirringwith stirring for 3 hours
3. stirringagain and the suspension was stirred at the same temperature for 12 hours
4. customthe mixture was quenched by sequential addition of water (1.3 ml), 15% aqueous sodium hydroxide (1.3 ml), water (3.8 ml)
5. stirringthe whole was stirred at room temperature for 2 hours
6. customThe resulting insoluble materials were removed by filtration
7. dry with materialthe filtrate was dried over sodium sulfate
8. customevaporated under reduced pressure