反应详情

3-Dimethylamino-5-pentafluorosulfanylbenzoic acid (1.0 g) was dissolved in methylene chloride (60 ml). Thionyl chloride (5 ml) was added with stirring and the mixture was stirred at RT for 2 h. To complete the reaction, it was subsequently heated at reflux for 3 h. After cooling, the solvent was stripped off, and the residue was dissolved in methylene chloride (50 ml), treated with N,O-dimethylhydroxylamine hydrochloride and Hünig's base (1 ml) was added. After stirring for one hour, the solvent was stripped off, and the residue was taken up with ethyl acetate and washed 5 times with water. The organic phase was dried with magnesium sulfate, filtered and concentrated. 980 mg of the title compound were obtained, which were reacted directly in the next stage.

1. stirringthe mixture was stirred at RT for 2 h
2. customthe reaction, it
3. temperaturewas subsequently heated
4. temperatureat reflux for 3 h
5. temperatureAfter cooling
6. additionwas added
7. stirringAfter stirring for one hour
8. washwashed 5 times with water
9. dry with materialThe organic phase was dried with magnesium sulfate
10. filtrationfiltered
11. concentrationconcentrated