反应详情

To a solution of 2,6-dichlorobenzaldehyde (880 mg, 5.03 mmol) in THF (10 mL) was added EtMgCl/THF (2.0 M, 3 mL, 6.0 mmol) at 0° C. under nitrogen, the resulting mixture was allowed to warm to rt and stirred at rt overnight. The mixture was quenched with sat. aq. NH4Cl (5 mL) at 0° C., then diluted with Et2O (50 mL), the organic phase was washed with brine (20 mL), and dried over anhydrous sodium sulfate. The residue was purified by silica gel chromatography (Hex:EtOAc=80:20) to give the title compound as a colorless oil. 1H NMR (CDCl3): δ=1.00 (t, J=7.4 Hz, 3H), 1.95-2.11 (m, 2H), 2.82 (d, J=10.4 Hz, 1H, —OH), 5.34 (m, 1H), 7.13 (t, J=7.6 Hz, 1H), 7.29 (d, J=7.8 Hz, 2H.)

1. customThe mixture was quenched with sat. aq. NH4Cl (5 mL) at 0° C.
2. additiondiluted with Et2O (50 mL)
3. washthe organic phase was washed with brine (20 mL)
4. dry with materialdried over anhydrous sodium sulfate
5. customThe residue was purified by silica gel chromatography (Hex:EtOAc=80:20)