反应详情

温度

0 °C

To a cooled (1.3° C.) mixture of 1-bromo-2,4,6-trifluorobenzene (30.0 g, 142 mmol) and H2SO4 (115 mL) was added HNO3 (68%, 102 mL) over 1.5 h at such a rate that the internal temperature was <8° C. After stirring at 0° C. for 2 h, the resulting mixture was poured into ice water (1850 mL), stirred vigorously for 30 min and extracted with CH2Cl2 (3×600 mL). The combined organic layers were washed with water (2×600 mL), dried over MgSO4, filtered and concentrated in vacuo to give the desired product as a clear yellow oil (35.0 g, 99% yield). 1H NMR (CDCl3) δ 7.01 (ddd, J=2.4, 7.8, 9.3 Hz, 1H); 19F NMR (CDCl3) δ −116.20 to −116.10, −107.73 to −107.71, −93.80 to −93.70.

1. temperatureTo a cooled
2. customwas <8° C
3. stirringstirred vigorously for 30 min
4. extractionextracted with CH2Cl2 (3×600 mL)
5. washThe combined organic layers were washed with water (2×600 mL)
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo