反应详情

温度

70 °C

A solution of 22 g (48.5 mmol) N-(2-benzyloxy-4-bromo-6-nitro-phenyl)-propionyl-propionamide, 4.9 g (30 mmol) iron(III) chloride and 7.2 g activated charcoal in 180 ml methanol was heated to 70° C. 23.8 ml (490 mmol) Hydrazine hydrate were added dropwise and the reaction mixture was refluxed for 90 min. After cooling to room temperature, the reaction was filtered through celite, the filter cake washed with dichloromethane, the filtrate reduced in volume and poured into water. The precipitate was filtered and washed with diethyl ether to afford 19 g (89%) of the title compound as a white solid.

1. temperaturethe reaction mixture was refluxed for 90 min
2. temperatureAfter cooling to room temperature
3. filtrationthe reaction was filtered through celite
4. washthe filter cake washed with dichloromethane
5. additionpoured into water
6. filtrationThe precipitate was filtered
7. washwashed with diethyl ether