反应详情

A mixture of 75 g (238 mmol) of 2-(2-nitrophenyl)-9,9-dimethyl-9H-fluorene and 290.3 ml (1669 mmol) of triethyl phosphite is heated under reflux for 12 h. The triethyl phosphite which remains is subsequently removed by distillation (72-76° C./9 mm Hg). Water/MeOH (1:1) is added to the residue, and the solid is filtered off and recrystallised. Yield: 61.3 g (216 mmol), 92%.

1. temperatureis heated
2. temperatureunder reflux for 12 h
3. customThe triethyl phosphite which remains is subsequently removed by distillation (72-76° C./9 mm Hg)
4. additionWater/MeOH (1:1) is added to the residue
5. filtrationthe solid is filtered off
6. customrecrystallised