反应详情

To a 0° C. suspension of 4′-hydroxy-2′-methylacetophenone (969 mg, 6.45 mmol), [3-(2,6-Dichloro-phenyl)-5-isopropyl-3H-[1,2,3]triazol-4-yl]-methanol (1.85 g, 6.45 mmol), tri-n-butylphosphine (2.42 ml, 9.73 mmol) in toluene (20 mL) is added ADDP (2.46 g, 9.73 mmol). The reaction mixture is warmed to room temperature and stirred overnight. The reaction mixture is concentrated and the residue is chromatographed eluting with 0% to 30% EtOAc/Hex to yield the title compound (1.71 mg, 63%). 1H NMR (400 MHz, CDCl3) δ 7.75 (dd, 1H, J=8.5, 2.1 Hz), 7.72 (d, 1H, J=1.3 Hz), 7.49 (d, 1H, J=2.2 Hz), 7.47 (s, 1H), 7.41 (dd, 1H, J=9.2, 6.6 Hz), 6.78 (d, 1H, J=8.4 Hz), 4.99 (s, 2H), 3.22 (sept, 1H, J=7.0 Hz), 2.52 (s, 3H), 2.06 (s, 3H), 1.46 (d, 6H, J=7.0 Hz).

1. concentrationThe reaction mixture is concentrated
2. customthe residue is chromatographed
3. washeluting with 0% to 30% EtOAc/Hex