反应详情

To a solution of 2-methylthio-6-nitrophenol (410 mg, 2.21 mmol) in acetic acid (15 ml) was added sodium perborate tetrahydrate (1.00 g, 6.50 mmol) and the mixture was stirred at room temperature for 2 hours. To the reaction solution was then added zinc powder (7 g, 0.107 mmol) with ice-cooling, and the mixture was stirred at room temperature for 1 hour. The reaction mixture was neutralized with a saturated sodium bicarbonate solution and extracted with chloroform. The organic layer was washed with a saturated sodium chloride solution, dried over anhydrous sodium sulfate and concentrated in vacuo. The resulting residue was purified by a silica gel column chromatography (silica gel 50 g, developing solvent; chloroform) to provide 234 mg (yield 62%) of 2-amino-6-methanesulfinylphenol as colorless amorphous.

1. stirringthe mixture was stirred at room temperature for 1 hour
2. extractionextracted with chloroform
3. washThe organic layer was washed with a saturated sodium chloride solution
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated in vacuo
6. customThe resulting residue was purified by a silica gel column chromatography (silica gel 50 g, developing solvent; chloroform)