反应详情

Water (5 mL) was chilled in an ice bath and nitrososulfuric acid was added dropwise. A suspension of 4-Bromo-2,6-dimethyl-benzamide (1.30 g, 5.23 mmol) in dichloromethane (10 mL) was added. The organic phase was dried over magnesium sulfate and concentrated. It was taken up in ethyl acetate and extracted three times with saturated sodium bicarbonate. The combined aqueous extracts were acidified with 6M hydrochloric acid and extracted three times with ethyl acetate. The combined organic extracts were washed with brine, dried over magnesium sulfate, filtered and concentrated to provide the title compound as a colourless solid (1.14 g, 88%). 1H NMR CDCl3: δ 7.48 (s, 1H), 7.35 (s, 1H), 2.45 (s, 3H).

1. additionwas added
2. dry with materialThe organic phase was dried over magnesium sulfate
3. concentrationconcentrated
4. extractionextracted three times with saturated sodium bicarbonate
5. extractionextracted three times with ethyl acetate
6. washThe combined organic extracts were washed with brine
7. dry with materialdried over magnesium sulfate
8. filtrationfiltered
9. concentrationconcentrated