反应详情

温度

40 °C

To a solution of 1-benzy-6-hydroxymethyl-4-methyl-6-nitrohexahydro-1H-1,4-diazepine in methanol (800 ml), potassium tert-butoxide (97 g) is added, and the solution is heated at about 40° C. for 30 minutes. The solvent is evaporated under reduced pressure, and the residue is diluted in a solution of hydroxylamine hydrochloride (60 g) in water (500 ml) and extracted with dichloromethane. The organic layer is washed with saturated aqueous sodium chloride solution and dried over magnesium sulfate. The solvent is evaporated under reduced pressure, and the residue is chromatographed on silica gel with elution of ethyl acetate. Fractions containing the object compound are pooled and evaporated under reduced pressure to give 1-benzyl-4-methyl-6-nitrohexahydro-1H-1,4-diazepine (45 g) as a pale yellow oil.

1. customThe solvent is evaporated under reduced pressure
2. additionthe residue is diluted in a solution of hydroxylamine hydrochloride (60 g) in water (500 ml)
3. extractionextracted with dichloromethane
4. washThe organic layer is washed with saturated aqueous sodium chloride solution
5. dry with materialdried over magnesium sulfate
6. customThe solvent is evaporated under reduced pressure
7. customthe residue is chromatographed on silica gel with elution of ethyl acetate
8. additionFractions containing the object compound
9. customevaporated under reduced pressure