反应详情

Method A2 Sodium hydride (148 mg) was added to dry DMSO (5.5 mL) and the mixture was stirred at RT for 20 minutes under Ar atmosphere. 4-amino-3-(methylthio)phenol (573 mg, 3.7 mmol) was added thereto, and the mixture stirred for 10 more minutes. Next, 4-Chloro-3-nitropyridin-2-amine (3.7 mmol) was added, and the mixture was heated to 100′C and stirred for 3 hours. After cooling down, water was added, and the mixture extracted three times with EtOAc. The combined organic layers were washed first with a saturated aqueous sodium hydrogen carbonate solution then water, dried over MgSO4 and evaporated to afford the title compound (657 mg, 61%) was obtained after purification by chromatography on silica gel (EtOAc-DCM, 1:1) as a red brown solid (Rf 0.56, EtOAc-DCM, 1:1).

1. stirringthe mixture stirred for 10 more minutes
2. temperaturethe mixture was heated to 100′C
3. stirringstirred for 3 hours
4. temperatureAfter cooling down
5. extractionthe mixture extracted three times with EtOAc
6. washThe combined organic layers were washed first with a saturated aqueous sodium hydrogen carbonate solution
7. dry with materialwater, dried over MgSO4
8. customevaporated