反应详情

1.00 g (5.06 mmol) of 3-chloro-5-nitro-1H-indazole was suspended in 50 ml of ethanol, and 5.71 g (25.3 mmol) of tin(II) chloride dihydrate were added. The mixture was left to stir at reflux overnight, saturated aqueous sodium bicarbonate solution was then added and the mixture was extracted three times with ethyl acetate. The combined organic phases were dried over magnesium sulphate and the solvent was removed under reduced pressure. The mixture was triturated with tert-butyl methyl ether and the solid was filtered off with suction. Yield: 544 mg (purity 90%, 58% of theory)

1. waitThe mixture was left
2. temperatureat reflux overnight
3. extractionthe mixture was extracted three times with ethyl acetate
4. dry with materialThe combined organic phases were dried over magnesium sulphate
5. customthe solvent was removed under reduced pressure
6. customThe mixture was triturated with tert-butyl methyl ether
7. filtrationthe solid was filtered off with suction