反应详情

Stir a mixture of 1-(2-Hydroxy-4-mercapto-3-propyl-phenyl)-ethanone (132 mg, 0.63 mmol), 3-(3-Iodomethyl-benzyl)-benzoic acid methyl ester (230 mg, 0.63 mmol), and cesium carbonate (410 mg, 1.26 mmol) in 2-butanone (6 ml) at room temperature under argon for 20 hours. Pour the mixture into water (60 ml) and extract with ethyl acetate (2×30 ml). Combine the organic extracts and wash with water, brine, then dry over sodium sulfate, filter and concentrate. Purify the crude product via silica chromatography eluting with 1:4 ethyl acetate:hexanes to give the title compound (240 mg, 85%). MS (m/z) 447 (M−H).

1. extractionextract with ethyl acetate (2×30 ml)
2. washCombine the organic extracts and wash with water, brine
3. dry with materialdry over sodium sulfate
4. filtrationfilter
5. concentrationconcentrate
6. customPurify the crude product via silica chromatography
7. washeluting with 1:4 ethyl acetate