反应详情

温度

10 °C

48 g (0.2 mole) of sodium sulfide containing water of crystallization (Na2S. 9H2O) were dissolved in 300 ml of methanol. 6.8 g (0.2 mole) of hydrogen sulfide were passed into this solution at 10° to 20°C and 32.7 g (0.1 mole) of 2-chloromethyl-3,4,5,6-tetrachlorobenzoyl chloride were then introduced at 20° to 30°C. The mixture was boiled for 6 hours under reflux and after cooling to 10°C was acidified to pH 5 with concentrated hydrochloric acid. The crystal paste which separated out was filtered off, and the residue was washed with water and acetone and dried. The yield was 27.5 g (representing 95.5% of theory) of almost colorless crystalline powder of melting point 181°-183°C.

1. customwater of crystallization (Na2S. 9H2O)
2. dissolutionwere dissolved in 300 ml of methanol
3. customwere passed into this solution at 10° to 20°C
4. temperatureunder reflux
5. customThe crystal paste which separated out
6. filtrationwas filtered off
7. washthe residue was washed with water and acetone
8. customdried