反应详情

To a stirred solution of 1-(6-bromo-2-pyridinyl)-1-pentanol (250 mg, 1.02 mmol) and ethyl (4-hydroxy-2-ethylphenoxy)acetate (230 mg, 1.02 mmol) in dry THF (21 mL) at 0° C. (ice/water bath) under nitrogen was added ADDP (517 mg, 2.04 mmol) followed by nBu3P (510 μL, 2.04 mmol) drop-wise. The mixture was stirred with slow warming to rt over 18 hours and then concentrated under vacuum, diluted with EtOAc (150 mL) and washed with water (3×75 mL), dried (MgSO4), filtered and reduced to give an oil. Purification by SPE (silica, 10 g Cartridge) eluting with cyclohexane:EtOAc (gradient 20:1 to 5:1) afforded the title compound (307 mg).

1. concentrationconcentrated under vacuum
2. additiondiluted with EtOAc (150 mL)
3. washwashed with water (3×75 mL)
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customto give an oil
7. customPurification by SPE (silica, 10 g Cartridge)
8. washeluting with cyclohexane