反应详情

温度

60 °C

To a solution of 2-chloro-5-iodo-4-methylbenzoic acid (Preparation 49, 2.50 g, 8.43 mmol) in methanol (50 mL) was added concentrated sulfuric acid (1.2 mL) and the reaction was heated at 60° C. for 18 hours. The reaction was cooled, concentrated in vacuo, diluted with water and basified with potassium carbonate until pH=9. The aqueous solution was extracted with EtOAc (3×100 mL), the organic layers combined, washed with water (100 mL), brine (100 mL), dried over magnesium sulphate and concentrated in vacuo to afford the title compound (2.3 g, 88%).

1. temperatureThe reaction was cooled
2. concentrationconcentrated in vacuo
3. additiondiluted with water
4. extractionThe aqueous solution was extracted with EtOAc (3×100 mL)
5. washwashed with water (100 mL), brine (100 mL)
6. dry with materialdried over magnesium sulphate
7. concentrationconcentrated in vacuo