反应详情

温度

60 °C

To a mixture of 2-nitro-5-propoxy-benzamide (1.20 g, 5.36 mmol) in MeOH-H2O (v/v, 3:1, 60 mL) was added NH4Cl (2.84 g, 53.6 mmol) and Fe (2.99 g, 53.6 mmol). The resulting mixture was stirred at 60° C. for 3 h. After the reaction was completed, the mixture was cooled to room temperature and the iron was filtered off. The filtrate was concentrated to 15 mL and the formed precipitate was collected and dried in vacuo to give 1.02 g of ii-a as a pale yellow solid (98%). LCMS m/z=1781 (M−16), 195.1 (M+1) (Method B) (retention time=1.46 min).

1. temperaturethe mixture was cooled to room temperature
2. filtrationthe iron was filtered off
3. concentrationThe filtrate was concentrated to 15 mL
4. customthe formed precipitate was collected
5. customdried in vacuo