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0 °C

To a mixture of pentafluorophenol (3.3 g, 17.96 mmol), 4-bromobutanoic acid (3.0 g, 17.96 mmol) and DMAP (0.440 g, 3.59 mmol) in CH2Cl2 (30 ml), cooled to 0° C., EDAC.HCl (5.2 g, 26.94 mmol) was added in portion. The mixture was then stirred at 0° C. for 30 minutes. Then it was gradually warmed to room temperature and stirred for 480 minutes. Then the mixture was diluted with NaH2PO4 aqueous (5%, 50 ml) and acidified with HCl 1N to pH 3-4. The organic phase was separated and the aqueous phase was extracted with CH2Cl2 (2×50 ml). The organic phase washed with brine, dried over Na2SO4 and evaporated to give an oil that was purified by flash chromatography (n-Hexane/EtOAc 98:2) to yield 4-bromobutanoic acid pentafluorophenyl ester (5.2 g, 86%) as a colorless oil.

1. temperatureThen it was gradually warmed to room temperature
2. stirringstirred for 480 minutes
3. customThe organic phase was separated
4. extractionthe aqueous phase was extracted with CH2Cl2 (2×50 ml)
5. washThe organic phase washed with brine
6. dry with materialdried over Na2SO4
7. customevaporated
8. customto give an oil that
9. customwas purified by flash chromatography (n-Hexane/EtOAc 98:2)