反应详情

A solution of tert-butyl (2-hydroxy-3-iodo-5-nitrophenyl)carbamate (1.0 g, 2.6 mmol) and N,N-carbonyldiimidazole (0.47 g, 2.9 mmol) in THF (6 mL) was stirred at reflux for 1 h. The reaction mixture was concentrated, diluted with ethyl acetate (100 mL), washed with 1 N HCl (50 mL), water (20 mL), and brine (20 mL), dried over anhydrous sodium sulfate, filtered, and concentrated to give a crude solid. This material was concentrated from hexanes (2×) to give the desired product (5.7 g, 91%) as an orange solid. This material was purified by flash column chromatography to give the desired product (0.66 g, 82%) as a yellow solid. LCMS for C7H41N2O4 (M+H)+: m/z=306.8.

1. temperatureat reflux for 1 h
2. concentrationThe reaction mixture was concentrated
3. additiondiluted with ethyl acetate (100 mL)
4. washwashed with 1 N HCl (50 mL), water (20 mL), and brine (20 mL)
5. dry with materialdried over anhydrous sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customto give a crude solid
9. concentrationThis material was concentrated from hexanes (2×)