反应详情

A solution of rac-2-(2,6-dimethyl-4-prop-1-ynylphenyl)-3-methoxy-5-pyridin-2-ylmethylcyclopent-2-enone (0.5 g, 1.45 mmol) in acetone (10 ml) and 2N hydrochloric acid (5 ml) is heated at 80°C. under microwave irradiation for 40 minutes. Volatile solvents are removed in vacuo and residue is diluted with distilled water (50 ml) and extracted with ethyl acetate (3×50 ml). The combined organic fractions are washed again with distilled water, brine, dried over sodium sulfate, filtered and the filtrate concentrated in vacuo. The crude product is purified by flash column chromatography to afford rac-2-(2,6-Dimethyl-4-prop-1-ynylphenyl)-4-pyridin-2-ylmethylcyclopentane-1,3-dione.

1. customVolatile solvents are removed in vacuo and residue
2. additionis diluted with distilled water (50 ml)
3. extractionextracted with ethyl acetate (3×50 ml)
4. washThe combined organic fractions are washed again with distilled water, brine
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationthe filtrate concentrated in vacuo
8. customThe crude product is purified by flash column chromatography