反应详情

In 20 ml of ethanol, 2.1 g (12.2 mmol.) of 2-methylthiobenzyl chloride, 2.17 g (12.3 mmol.) of methyl 1-piperazinecarbodithioate and 1.30 g (12.3 mmol.) of sodium carbonate were refluxed under heating for 2 hours. Ethanol was distilled off under reduced pressure. The residue was extracted with ether, after addition of water. The ether portion was washed with water and a saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate, and placed under reduced pressure to distill off the solvent. The residue was purified over silica gel column, to give 1.18 g of the desired compound as a yellow oil, yield 31%.

1. temperatureunder heating for 2 hours
2. distillationEthanol was distilled off under reduced pressure
3. extractionThe residue was extracted with ether
4. additionafter addition of water
5. washThe ether portion was washed with water
6. dry with materiala saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate
7. distillationto distill off the solvent
8. customThe residue was purified over silica gel column