反应详情

温度

50 °C

A suspension of 5-Chloro-N-(2-chloro-4-nitrophenyl)-2-hydroxybenzamide (1.27 g., 3.88 mmol) in pyridine (15 mL) was treated with 4-dimethylaminopyridine (30 mg) and benzoyl chloride (0.49 mL, 4.27 mmol) was introduced dropwise. The suspension was warmed to 50° C. for one hour then cooled to room temperature and stirred for 17 hours. The reaction mixture was partitioned between 1N aqueous HCl and ethyl acetate. The ethyl acetate phase was washed with water, then brine, dried over magnesium sulfate, and concentrated to an off-white solid. This was recrystallized from ethyl acetate/hexanes. 1HNMR (500 MHz, DMSO-d6): δ7.70 (M, 3H), 7.73 (m, 2H), 7.89 (m, 1H), 7.93 (M, 1H), 8.19 (m, 1H), 8.32 (m, 1H), 10.60 (s, 1H).

1. additionwas introduced dropwise
2. temperaturethen cooled to room temperature
3. customThe reaction mixture was partitioned between 1N aqueous HCl and ethyl acetate
4. washThe ethyl acetate phase was washed with water
5. dry with materialbrine, dried over magnesium sulfate
6. concentrationconcentrated to an off-white solid
7. customThis was recrystallized from ethyl acetate/hexanes