反应详情

To a solution of this aminophenol. (233 mg, 1.36 mmol) in ethanol (10 ml) was added potassium O-ethyl dithiocarbonate (300 mg, 1.87 mmol) and the mixture was stirred under heating to reflux for 9 hours. The reaction solution was acidified to pH, 4 with 1 N hydrochloric acid and extracted with chloroform. The organic layer was washed with a saturated sodium chloride solution, dried over anhydrous sodium sulfate and concentraed in vacuo. The resulting residue was purified by a silica gel preparative thin layer chromatography (developing solvent; chloroform:methanol=10:1) and recrystallized from chloroform-ether to provide 223 mg (yield 77%) of 2-mercapto-7-methansulfinylbenzoxazole as pale brown powdery crystals.

1. temperatureunder heating
2. temperatureto reflux for 9 hours
3. extraction4 with 1 N hydrochloric acid and extracted with chloroform
4. washThe organic layer was washed with a saturated sodium chloride solution
5. dry with materialdried over anhydrous sodium sulfate
6. customThe resulting residue was purified by a silica gel preparative thin layer chromatography (developing solvent; chloroform:methanol=10:1)
7. customrecrystallized from chloroform-ether