反应详情

温度

140 °C

110 g (1.48 mol) of sodium hydrogen sulphide (NaSH·H2O) are initially introduced together with 1 l of N-methylpyrrolidone and the water is removed at 160° C. with nitrogen. The mixture is cooled to 140° C. and 112 g (0.59 mol) of 3,4-dichloroacetophenone are added, and the mixture is reacted further at 160° C. for 3 hours, and N-methylpyrrolidone is distilled off. The residue is taken up in 1 l of water and filtered, and the filtrate is acidified at 0°-10° C. with half-concentrated hydrochloric acid. The precipitate is filtered off with suction, washed neutral and dried. Distillation under reduced pressure gives 99.8 g (90.7% of theory) of 2-chloro-4-acetylthiophenol of boiling point: 125°-130° C./0.1 mbar.

1. customthe water is removed at 160° C. with nitrogen
2. customthe mixture is reacted further at 160° C. for 3 hours
3. distillationN-methylpyrrolidone is distilled off
4. filtrationfiltered
5. customis acidified at 0°-10° C. with half-concentrated hydrochloric acid
6. filtrationThe precipitate is filtered off with suction
7. washwashed neutral
8. customdried
9. distillationDistillation under reduced pressure