反应详情

3.22 g (9.1 mmol) of the compound from Example 86 dissolved in 50 ml of absolute tetrahydrofuran are added dropwise at 0° C. to a solution of 2.11 g (18.2 mmol) of sodium phenoxide 50 ml of absolute tetrahydrofuran and the mixture is heated to reflux for 4 days. After cooling to room temperature, the mixture is diluted using 150 ml of water and extracted several times using ether. The combined organic phases are dried over magnesium sulphate and concentrated in vacuo, and the residue chromatographed on a column (silica gel 70-230 mesh, using petroleum ether/ethyl acetate 95.5).

1. temperaturethe mixture is heated
2. temperatureto reflux for 4 days
3. additionthe mixture is diluted
4. extractionextracted several times
5. dry with materialThe combined organic phases are dried over magnesium sulphate
6. concentrationconcentrated in vacuo
7. customthe residue chromatographed on a column (silica gel 70-230 mesh, using petroleum ether/ethyl acetate 95.5)