反应详情

3-Acetamino-4-fluoro-6-methyl-phenylsulfonylchloride (500 g, 1.89 mol) was dissolved in 2 L of acetic acid. Red phosphorus (100 g, 3.22 mmol) and iodine (10 g, 39 mmol) were added to the solution, and the mixture was refluxed for 3 hours. The acetic acid was removed under reduced pressure, water was added and the residue extracted with ethyl acetate. The organic phase was dried with sodium sulfate and concentrated under reduced pressure to give 5-acetamino-4-fluoro-2-methyl-benzenethiol as a crude intermediate (270 g, 72%).

1. temperaturethe mixture was refluxed for 3 hours
2. customThe acetic acid was removed under reduced pressure, water
3. additionwas added
4. extractionthe residue extracted with ethyl acetate
5. dry with materialThe organic phase was dried with sodium sulfate
6. concentrationconcentrated under reduced pressure