反应详情

温度

60 °C

A solution D8 (1 g, 7 mmol) in sulfuric acid (2.5 ml) was cooled (<4° C.) and concentrated nitric acid (1 ml) added over 10 min. Reaction was stirred for 30 min and then heated at 60° C. for 2 h. After cooling the reaction mixture was poured into ice water slurry (100 ml) and basified using solid potassium carbonate followed by extraction using DCM. Organic phase was separated, dried over MgSO4, filtered and concentrated under reduced pressure to afford the title compound as a white solid.

1. additionadded over 10 min
2. customReaction
3. temperatureAfter cooling the reaction mixture
4. extractionfollowed by extraction
5. customOrganic phase was separated
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure