反应详情

In a nitrogen atmosphere, 5.615 g (30.08 mmol.) of 3,4-dimethoxybenzyl chloride, 5.57 g (30.08 mmol., purity 95%) of methyl 1-piperazinecarbodithioate, 3.19 g (30.08 mmol.) of anhydrous sodium carbonate and 50 ml of ethanol were mixed and refluxed under heating for 5.5 hours. The solvent was distilled off under reduced pressure. To the residue were added 20 ml of dichloromethane and 20 ml of water. The organic solvent portion was taken out and washed with 30 ml of 1-N hydrochloric acid. To the organic portion was added 1-N aqueous sodium hydroxide solution. The organic solvent portion was again taken out and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. To the residue was added 20 ml of ethanol. Precipitated crystals were collected by filtration and washed with ethanol to give 1.465 g of methyl 4-(3,4-dimethoxybenzyl)-1-piperazinecarbodithioate, yield 14.9%.

1. temperaturerefluxed
2. temperatureunder heating for 5.5 hours
3. distillationThe solvent was distilled off under reduced pressure
4. additionTo the residue were added 20 ml of dichloromethane and 20 ml of water
5. washwashed with 30 ml of 1-N hydrochloric acid
6. additionTo the organic portion was added 1-N aqueous sodium hydroxide solution
7. dry with materialdried over anhydrous sodium sulfate
8. distillationThe solvent was distilled off under reduced pressure
9. additionTo the residue was added 20 ml of ethanol
10. customPrecipitated crystals
11. filtrationwere collected by filtration
12. washwashed with ethanol