反应详情

2-Nitropropane (7.7 ml) and compound C (20.0 g) were added to a solution of sodium (1.52 ) in ethanol (80 ml) and the solution was heated under reflux for 5 hours. Volatile material was removed by evaporation and the residue was partitioned between ether (300 ml) and water (300 ml). The organic phase was separated, washed with saturated sodium chloride solution and dried (MgSO4). The solvent was removed by evaporation and the residue was purified by flash chromatography, eluting with a mixture of ethyl acetate and hexane (1:9 v/v gradually changing to 1:1 v/v), to give methyl 4'-formylbiphenyl-2-carboxylate (D) (10.2 g) as a waxy solid; NMR (d6 -DMSO): 3.6(s,3H), 7.45-7.6(m,4H), 7.7(d of t, 1H), 7.85(d of d, 1H), 7.95(d,2H), 10.05(s,1H).

1. temperaturethe solution was heated
2. temperatureunder reflux for 5 hours
3. customVolatile material was removed by evaporation
4. customthe residue was partitioned between ether (300 ml) and water (300 ml)
5. customThe organic phase was separated
6. washwashed with saturated sodium chloride solution
7. dry with materialdried (MgSO4)
8. customThe solvent was removed by evaporation
9. customthe residue was purified by flash chromatography
10. washeluting with a mixture of ethyl acetate and hexane (1:9 v/v