反应详情

6.80 g of sodium dithionite was added to a mixture of 1.23 g of 5-(4-methoxy-phenyl)-3-methyl-4-nitroso-1H-pyrazole (Example 22(c)) and 50 ml of water at 70° C., and the reaction mixture was stirred for 15 minutes. 5 ml of ethanol was added and the reaction mixture was stirred for 10 minutes. The reaction mixture was extracted with ethyl acetate. The organic layer was washed with brine, dried over magnesium sulfate, filtered and concentrated. Trituration with ether gave the title compound as a beige solid, melting point 120–122° C., C11H13N3O (203.24), MS (ESI, method B) 204 (M+H).

1. stirringthe reaction mixture was stirred for 10 minutes
2. extractionThe reaction mixture was extracted with ethyl acetate
3. washThe organic layer was washed with brine
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated