反应详情

To a CH2Cl2 (210 mL) solution of 4-fluorophenyl acetic acid (32.28 g, 209.42 mmol) at 0° C. was added DMAP (25.58 g, 209.42 mmol), and Meldrum's Acid (30.18 g, 209.42 mmol) followed by DCC (43.21 g, 209.42 mmol). The reaction mixture was warmed to ambient temperature and stirred for 4 h. The reaction was filtered to remove the DCU and the filtrate washed with 1N HCl, H2O, and brine. The organics were dried (Na2SO4), filtered and concentrated to a yellow oil. The residue was redissolved in THF (200 mL) and allyl alcohol (14.38 mL, 211.51 mmol). The reaction mixture was refluxed for 3 h and then concentrated to deliver 47 g (95% yield) of the title compound as a pale yellow oil and used without further purification.

1. filtrationThe reaction was filtered
2. customto remove the DCU
3. washthe filtrate washed with 1N HCl, H2O, and brine
4. dry with materialThe organics were dried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated to a yellow oil
7. dissolutionThe residue was redissolved in THF (200 mL)
8. temperatureThe reaction mixture was refluxed for 3 h
9. concentrationconcentrated