反应详情

To 20 ml of ethanol was 1.05 g of 37% formalin, and to the mixture was added under chilling with ice 2.29 g of methyl 1-piperazinecarbodithioate. The mixture was then stirred for 30 min. at room temperature, and, after addition of 1.24 g of 4-methoxyphenol, refluxed overnight under heating. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography. The obtained oil was crystallized from 10 ml of ethanol. The crystals were collected by filtration and subsequently washed with ethanol to give 1.06 g of the desired compound as white crystals, m.p. 112° C., yield 34%.

1. additionto the mixture was added
2. temperaturerefluxed overnight
3. temperatureunder heating
4. distillationThe solvent was distilled off under reduced pressure
5. customthe residue was purified by silica gel column chromatography
6. customThe obtained oil was crystallized from 10 ml of ethanol
7. filtrationThe crystals were collected by filtration
8. washsubsequently washed with ethanol