反应详情

A stirred solution of 2.54 g (0.01 mol) of 2-(6,11-dihydro-11-oxodibenz[b,e]oxepin-2-yl)ethanol of Example 1, 20 ml of sieve dried CH2Cl2 and 1.55 g (0.013 mol) of phenylisocyanate was heated 20 hours under reflux with exclusion of moisture. The cooled solution was concentrated on a rotary evaporator to afford an oil which was dissolved in 10 ml of hot toluene. The solution was seeded with product (previously obtained by the method described herein), stirred until a thick suspension formed and allowed to stand overnight (about 16 hours) at ambient temperature. Filtration and drying in vacuo afforded 2.53 g (67.8%) of a colorless solid of 2-(6,11-dihydro-11-oxodibenz[b,e]oxepin-2-yl)ethyl carbanilate m.p. 98°-99° C.

1. temperatureunder reflux with exclusion of moisture
2. concentrationThe cooled solution was concentrated on a rotary evaporator
3. customto afford an oil which
4. custompreviously obtained by the method
5. customformed
6. custom(about 16 hours)
7. customat ambient temperature
8. filtrationFiltration
9. customdrying in vacuo