反应详情

温度

20 °C

42.3 g of 6-amino-5-nitro-nicotinamide (0.23 mol, HPLC: 93% area) was suspended in methanol/water 1:1 (500 mL). 5.2 g of catalyst [Pd(5%)/C (57.8% H2O); type: 39, Johnson Matthey] was added. Hydrogenation was carried out at 5 bar and 30° C. for 4 h. After completion the catalyst was filtered off and washed with methanol/water 1/1 (100 mL). 550 mL of the solvent was distilled off. The resulting suspension was cooled to 20° C. and filtered off. The solid was washed with methanol (20 mL) and TBME (30 mL). After drying (200-10 mbar; 40° C. bath temperature, 16 b) 28.5 g of the title compound (0.18 mol, 78%) was obtained.

1. filtrationAfter completion the catalyst was filtered off
2. washwashed with methanol/water 1/1 (100 mL)
3. distillation550 mL of the solvent was distilled off
4. filtrationfiltered off
5. washThe solid was washed with methanol (20 mL) and TBME (30 mL)