反应详情

4-hydroxybenzylamine hydrate, prepared as above (5.33 g) and N,N'-Bis(tert-butoxycarbonyl)-S-methylisothiourea (10.96 g) were combined in 150 mL THF, and stirred at reflux for 4 hr. The mixture was concentrated, and the crude product chromatographed on silica gel with 10% ethyl acetate in dichloromethane. Recrystallization from methanol-water provided the title compound as a white solid, mp 187°-189° C. (10 g, 70%).

1. temperatureat reflux for 4 hr
2. concentrationThe mixture was concentrated
3. customthe crude product chromatographed on silica gel with 10% ethyl acetate in dichloromethane
4. customRecrystallization from methanol-water