反应详情

6-(S-Trityl-)mercaptohexylphthalimide (14.27 g, 28.2 mmol) was suspended in ethanol (250 mL). Hydrazine hydrate (3.45 mL, 70.5 mmol) was added, and the mixture was heated to reflux for 2 h. The mixture was filtered and the filtrate was concentrated in vacuo. Chloroform (180 mL) was added to the residual oil and the resulting suspension was stirred at room temperature for 1.5 h. The mixture was filtered, and the filtrate was extracted with water (60 mL) and brine (60 mL), dried over MgSO4 and concentrated to yield crude 6-(tritylmercapto)-hexylamine (10.10 g, 26.87 mmol, 95%).

1. temperaturethe mixture was heated
2. temperatureto reflux for 2 h
3. filtrationThe mixture was filtered
4. concentrationthe filtrate was concentrated in vacuo
5. additionChloroform (180 mL) was added to the residual oil
6. filtrationThe mixture was filtered
7. extractionthe filtrate was extracted with water (60 mL) and brine (60 mL)
8. dry with materialdried over MgSO4
9. concentrationconcentrated