反应详情

温度

80 °C

A mixture of 1.0 g of 9-trimethylsilyl-9-fluorenemethanol and 0.4 mL of phenyl isocyanate in 2.0 mL of dry benzene was heated in an oil bath at 80° C. for seven hours. The mixture was cooled to room temperature and triturated with 20 mL of Skelly F. The crystals deposited were removed by filtration, rinsed with Skelly F, and recrystallized from Skelly B to give 1.31 g (91.9%) of the urethane as white crystals, m.p. 137°-138° C.; IR(KBr): 3300 (NH), 1700 (C=O) cm-1 ; 1H NMR (CDCl3) 5 -0.12 (s, 9H, SiMe3), 5.07 (s, 2H, CH2), 6.21 (b, 1H, NH), 6.80-8.00 (m, 13H, aryl).

1. temperatureThe mixture was cooled to room temperature
2. customtriturated with 20 mL of Skelly F
3. customThe crystals deposited were removed by filtration
4. washrinsed with Skelly F
5. customrecrystallized from Skelly B