反应详情

温度

0 °C

The N-(2-hydroxy-3-aminophenyl)-N'-(2-bromophenyl)urea(274 mg, 0.85 lmmol) was added to HCl/H2O (0.85 mL/1.7 mL), cooled to 0° C. Sodium nitrate (58.6 mg, 0.85 mmol) was added to the reaction mixture. The reaction mixture was stirred at 0° C. for 30 minutes. Sodium azide (55 mg, 0.85 mmol) was added to reaction mixture and it was warmed to room temperature. The reaction mixture was stirred at room temperature for 18 hours then it was extracted with three times with ethyl acetate. The organic extracts were combined, dried over MgSO4, filtered and concentrated under reduced pressure and chromatography of the resulting solid on silica gel (hexane: ethyl acetate; 5:1) gave product (210 mg, 71%). EI-MS m/z 349 (M+H)+.

1. temperaturewas warmed to room temperature
2. stirringThe reaction mixture was stirred at room temperature for 18 hours
3. extractionit was extracted with three times with ethyl acetate
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure and chromatography of the resulting solid on silica gel (hexane: ethyl acetate; 5:1)