反应详情

Ethanol (4.6 g) was added to a fine suspension of sodium metal (2.25 g) in dry ether (200 ml) under an atmosphere of nitrogen. The mixture was heated for 8 hours, after which dibenzylphosphite (25.7 g) in dry ether (50 ml) was added. After standing over-night the dibenzylphosphite sodium salt was added over a period of 2 hours to a cold solution of ethyl chloroformate (10.8 g) in ether, under an atmosphere of nitrogen. The reaction was heated at reflux for 1 hour, cooled, washed with water, a NaCl solution and dried over Na2SO4. The ether was evaporated. After evaporating and discarding components volatile at 0.01 mm and 150° C. the residue was collected (13 g).

1. temperatureThe mixture was heated for 8 hours
2. waitAfter standing over-night
3. temperatureThe reaction was heated
4. temperatureat reflux for 1 hour
5. temperaturecooled
6. washwashed with water
7. dry with materiala NaCl solution and dried over Na2SO4
8. customThe ether was evaporated
9. customAfter evaporating
10. customvolatile at 0.01 mm and 150° C.
11. customwas collected (13 g)