反应详情

温度

80 °C

To a solution of 3,5-dimethyl-4-nitro-benzoic acid (10.0 g, 0.0512 mol) in MeOH (150 mL) is added thionyl chloride (10 ml) at 0° C. and the reaction is heated to 80° C. After 16 h, the reaction mixture is cooled to room temperature and solvent is removed under reduced pressure. The residue is diluted with water (50 ml) and basified with saturated NaHCO3 solution to pH 7-8 and extracted with EtOAc (2×120 mL). The organic layers are combined and dried over anhydrous sodium sulfate. The solvent is removed under reduced pressure to afford the title compound as a light yellow solid (10.71 g, 98.3%). 1H NMR (400 MHz, DMSO): δ 7.83 (s, 2H), 3.88 (s, 3H), 2.30 (s, 6H).

1. temperaturethe reaction mixture is cooled to room temperature
2. customsolvent is removed under reduced pressure
3. additionThe residue is diluted with water (50 ml)
4. extractionextracted with EtOAc (2×120 mL)
5. dry with materialdried over anhydrous sodium sulfate
6. customThe solvent is removed under reduced pressure