反应详情

A mixture of [2-(2,2-diethoxyethoxyl)pent-4-en-1-yl]cyclopropane (C66) (20 g, 83 mmol), aqueous hydrochloric acid (2 M, 83 mL, 166 mmol) and tetrahydrofuran (250 mL) was stirred at reflux for 1 hour. The reaction mixture was cooled to room temperature and concentrated to remove tetrahydrofuran. The aqueous phase was extracted with ethyl acetate (2×100 mL). The combined organic extracts were washed with saturated aqueous sodium chloride solution (3×50 mL), dried over sodium sulfate, filtered, and concentrated in vacuo to afford the product as a colorless oil (17 g). This material was taken directly into the following step.

1. temperatureat reflux for 1 hour
2. concentrationconcentrated
3. customto remove tetrahydrofuran
4. extractionThe aqueous phase was extracted with ethyl acetate (2×100 mL)
5. washThe combined organic extracts were washed with saturated aqueous sodium chloride solution (3×50 mL)
6. dry with materialdried over sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated in vacuo