反应详情

To a solution of 1a (4 gm, 7.54 mmol) in ethanol (40 mL), 20% KOH solution (10 mL) was added. The reaction mixture was refluxed for 2 h. Ethanol was evaporated under a vacuo, and was neutralized by 6 N HCL. The combined mixture was extracted in EtOAc (3×20 mL), washed with brine solution (20 mL). The organic layer was dried over Na2SO4 and evaporated to dryness. The crude residue was purified by silica gel column chromatography using 30% ethyl acetate in hexane as eluent to obtain pure compound 3,4,5-tris(benzyloxy)benzoic acid (1b) as white solid (2.78 g, 84%). Rf=0.515 (50% ethyl acetate in hexane)

1. temperatureThe reaction mixture was refluxed for 2 h
2. customEthanol was evaporated under a vacuo
3. extractionThe combined mixture was extracted in EtOAc (3×20 mL)
4. washwashed with brine solution (20 mL)
5. dry with materialThe organic layer was dried over Na2SO4
6. customevaporated to dryness
7. customThe crude residue was purified by silica gel column chromatography