反应详情

To a solution of 1-(4′-chloro-4-biphenylyl)-1-pentanol (140 mg, 0.51 mmol) in dry THF (15 mL) under nitrogen at 0° C. (ice/water bath) was added nBu3P (250 μL, 1.02 mmol), followed by ethyl (4-hydroxy-2-methylphenoxy)acetate (110 mg, 0.52 mmol) and ADDP (260 mg, 1.03 mmol) portion-wise. After stirring the mixture for 18 hours at rt under nitrogen the solvent was removed under vacuum. The residue was partitioned between water and EtOAc and extracted with EtOAc (3×30 mL). The organic extract was separated and dried (MgSO4) and the solvent removed under vacuum. Purification by flash chromatography (silica) eluting with cyclohexane:EtOAc (9:1) afforded the title compound as a colourless gum (150 mg).

1. customwas removed under vacuum
2. customThe residue was partitioned between water and EtOAc
3. extractionextracted with EtOAc (3×30 mL)
4. extractionThe organic extract
5. customwas separated
6. dry with materialdried (MgSO4)
7. customthe solvent removed under vacuum
8. customPurification by flash chromatography (silica)
9. washeluting with cyclohexane:EtOAc (9:1)