反应详情

To 5 ml of chloroform were added 152 mg of 4-acetoxyphenol, 211 mg of methyl 1-piperazinecarbodithioate and 36 mg of paraformaldehyde. The resulting mixture was refluxed for 4 hours. The mixture was cooled, and tothis was added chloroform. The mixture was then washed with water and a saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate and placed under reduced pressure to distill of the solvent. The residue was purified by siica gel column chromatography to yield an oil. The oil was crystallized by addition of ethanol. The obtained crystals were collected by filtration to give 224 mg of the desired compound as a white crystalline product, m.p. 124° C., yield 65.9%.

1. temperatureThe resulting mixture was refluxed for 4 hours
2. temperatureThe mixture was cooled
3. washThe mixture was then washed with water
4. dry with materiala saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate
5. distillationto distill of the solvent
6. customThe residue was purified by siica gel column chromatography
7. customto yield an oil
8. customThe oil was crystallized by addition of ethanol
9. filtrationThe obtained crystals were collected by filtration