反应详情

Dimethyl 2-hept-6-enylpropan-1,3-dioate(5 g, 21.9 mmol) prepared in Step 3 was dissolved in anhydrous DMSO(50 ml), 60% sodium hydride(0.96 g, 24.09 mmol) was added at room temperature, and the resulting mixture was stirred for 30 minutes at room temperature. To the reaction mixture was added 1,1,1,2,2-pentafluoro-8-iodooctane(8.7 g, 26.28 mmol) prepared in Step 2, which was then stirred overnight under heating at 70˜80° C. The temperature was lowered to 0° C. and water was added. The mixture thus obtained was extracted with ethyl acetate, washed with water and saturated saline solution in order, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by column chromatography(eluent:n-hexane/ethyl acetate=30/1, v/v) to give 9.3 g(Yield 98.8%) of the pure title compound as a colorless oil.

1. stirringwas then stirred overnight
2. temperatureunder heating at 70˜80° C
3. customwas lowered to 0° C.
4. customThe mixture thus obtained
5. extractionwas extracted with ethyl acetate
6. washwashed with water and saturated saline solution in order
7. dry with materialdried over anhydrous magnesium sulfate
8. concentrationconcentrated under reduced pressure
9. customThe residue was purified by column chromatography(eluent