反应详情

Into 1 l. r.b. flask equipped with a Dean Stark trap was placed 65 g (0.16 mole) of 1-(3',4'-dimethoxyphenyl)-7-(4'-chlorophenyl)-2-nitro-5-heptanone, 2 g p-toluenesulfonic acid, 100 ml ethylene glycol and 400 ml of cyclohexane. The mixture was allowed to reflux overnight, then concentrated in vacuo. Dil NaHCO3 solution was added to the residue and extracted with methylene chloride. The organic layer was backwashed with water, dried over anh MgSO4, filtered and concentrated under reduced pressure to obtain 45.3 g of an oil which solidified on drying at room temperature under vacuum.

1. customflask equipped with a Dean Stark trap
2. temperatureto reflux overnight
3. concentrationconcentrated in vacuo
4. additionDil NaHCO3 solution was added to the residue
5. extractionextracted with methylene chloride
6. dry with materialdried over anh MgSO4
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure