反应详情

1,2,3-Trifluoro-4-nitrobenzene (30 g, 0.17 mol), benzyl alcohol (18.4 g, 0.17 mol) and K2CO3 (35 g, 0.25 mol) were combined in DMF (300 mL) and were stirred at RT for 8 h. Water (300 mL) was added, and the mixture was extracted with EtOAc (3×500 mL). The combined organic layers were washed with brine, dried (MgSO4), concentrated in vacuo and purified by column chromatography on silica gel to give 1-benzyloxy-2,3-difluoro-4-nitrobenzene (16 g, 36% yield). 1H NMR (400 MHz, DMSO-d6): δ 8.06 (m, 1H), 7.49-7.30 (m, 6H), 5.37 (s, 2H).

1. extractionthe mixture was extracted with EtOAc (3×500 mL)
2. washThe combined organic layers were washed with brine
3. dry with materialdried (MgSO4)
4. concentrationconcentrated in vacuo
5. custompurified by column chromatography on silica gel