反应详情

温度

70 °C

A suspension of 2,6-dinitrophenol (5 g), ammonia (3 ml) and ammonium chloride (14.30 g) in water (30 ml) was heated to 70° C. A solution of sodium sulphide nonahydrate (24.19 g) in water (23 ml) was added and the resulting mixture stirred at 70° C. for 2 hours. The reaction was cooled to room temperature, acidified (pH 3.2) with 2N HCl, and the brown precipitate separated by filtration. The filtrate was extracted with chloroform (6×75 ml), the organic extracts combined with the precipitate, and evaporated in-vacuo to yield a dark brown solid. The solid was purified by flash chromatography (SiO2; dichloromethane) to yield the title compound (2.86 g, 68%) as a brown solid.

1. temperatureThe reaction was cooled to room temperature
2. customthe brown precipitate separated by filtration
3. extractionThe filtrate was extracted with chloroform (6×75 ml)
4. customevaporated in-vacuo
5. customto yield a dark brown solid
6. customThe solid was purified by flash chromatography (SiO2; dichloromethane)