反应详情

To a stirred solution of 3′-Hydroxyacetophenone (4.84 g, 35.5 mmol) in anhydrous CH2Cl2 (50 ml) was added at room temperature pyridine (25 ml) followed by addition of 2,6-Dimethylbenzoyl chloride (Step A, 6 g, 35 mmol) in anhydrous CH2Cl2 (10 ml) under argon. The reaction mixture was stirred for 16 hours, concentrated under reduced pressure, diluted with CH2Cl2, and washed with 0.1M HCl, water and brine. The organic layer was dried over Na2SO4, concentrated and purified by flash chromatography eluted with ethyl acetate:hexane (1:2) to give the title compound.

1. concentrationconcentrated under reduced pressure
2. additiondiluted with CH2Cl2
3. washwashed with 0.1M HCl, water and brine
4. dry with materialThe organic layer was dried over Na2SO4
5. concentrationconcentrated
6. custompurified by flash chromatography
7. washeluted with ethyl acetate:hexane (1:2)