反应详情

温度

80 °C

Alternatively a solution of N-(4-methyl-3-nitro-phenyl)-4-(4-methyl-piperazin-1-ylmethyl)-benzamide (60 g, 163 mmol) in ethanol 90% (300 ml) at room temperature under an atmosphere of nitrogen is treated sequentially with platinum (5%) on carbon (6.0 g) and potassium formate (68.5 g, 814 mmol). The resulting suspension is then heated at 80° C. for a period of 16 hrs. The reaction mixture is filtrated at 70° C. over a pad of Celite. Ethanol 90% (150 ml) and water (150 ml) are used to rinse the reactor. Ethanol is removed from the combined filtrates by distillation in vacuo at an external temperature 60° C. The crude product separates from the aqueous concentrate as an oil during the distillation, crystallizes upon subsequent cooling to 23° C. within 2 hrs and is filtered of with suction, washed with ethanol (200 ml) and dried in vacuo. Yield: 55 g of the title compound, 99% of theory, as yellowish crystals. (HPLC: 98.0% area).

1. filtrationThe reaction mixture is filtrated at 70° C. over a pad of Celite
2. washto rinse the reactor
3. customEthanol is removed from the combined filtrates by distillation in vacuo at an external temperature 60° C
4. concentrationThe crude product separates from the aqueous concentrate as an oil during the distillation
5. customcrystallizes
6. temperatureupon subsequent cooling to 23° C. within 2 hrs
7. filtrationis filtered of with suction
8. washwashed with ethanol (200 ml)
9. customdried in vacuo