反应详情

2-Bromo-5-(methylamino)-4-nitropyridine 1-oxide (10.0 g, 40.4 mmol) in 200 mL dichloromethane was mixed with phosphorous tribromide (10 mL, 106 mmol) in 50 mL dichloromethane at 10° C. and stirred for 10 minutes at ambient temperature. Water and methanol were added and the mixture was extracted with dichloromethane. The organic layers were washed with Na2CO3 (aq.) dried over MgSO4. The residue was triturated with ethanol, filtered and dried at 50° C. i. vac.

1. extractionthe mixture was extracted with dichloromethane
2. washThe organic layers were washed with Na2CO3 (aq.)
3. dry with materialdried over MgSO4
4. customThe residue was triturated with ethanol
5. filtrationfiltered
6. customdried at 50° C. i