反应详情

温度

150 °C

A mixture of 4-chloro-2-dimethoxymethyl-1-nitrobenzene (11.55 g, 0.0500 mol), phenol (4.70 g, 0.0500 mol), and potassium carbonate (8.16 g, 0.0600 mol) in DMA (100 mL) was stirred at 150° C. for 6 h. After cooling, the reaction mixture was poured into water and treated with diisopropyl ether. The organic layer was separated, washed with 10% aqueous KOH solution, dried (MgSO4), filtered, and concentrated. The resulting residue was purified by column chromatography on silica gel using as eluent CH2Cl2:petroleum ether (40:60, 60:40, 100:0 gradient). The product containing fractions were combined and evaporated to yield a residue which was dissolved in CH2Cl2 and washed with 10% aqueous KOH solution to remove the remaining phenol. Drying and evaporation yielded a residue.

1. temperatureAfter cooling
2. customThe organic layer was separated
3. washwashed with 10% aqueous KOH solution
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated
7. customThe resulting residue was purified by column chromatography on silica gel using as eluent CH2Cl2:petroleum ether (40:60, 60:40, 100:0 gradient)
8. additionThe product containing fractions
9. customevaporated
10. customto yield a residue which
11. washwashed with 10% aqueous KOH solution
12. customto remove the remaining phenol
13. customDrying
14. customevaporation
15. customyielded a residue