反应详情

To a solution of 4.257 g (25 mmol) of ω-undecylenyl alcohol in 25 mL of dry tetrahydrofuran was added 2.1 mL of pyridine (26.5 mmol) followed by dropwise addition of 3.10 mL of 2-bromoisobutyryl bromide (25 mmol) over 5 min. The mixture was stirred at room temperature overnight and then diluted with hexane (50 mL) and washed with 2 N HCl and twice with water. The organic phase was dried over sodium sulfate and filtered. The solvent was removed from the filtrate under reduced pressure, and the colorless oily residue was purified by flash column chromatography (hexane/ethyl acetate 25/1 v/v) to give 7.34 g (92%) of the ester as a colorless oil.

1. washwashed with 2 N HCl and twice with water
2. dry with materialThe organic phase was dried over sodium sulfate
3. filtrationfiltered
4. customThe solvent was removed from the filtrate under reduced pressure
5. customthe colorless oily residue was purified by flash column chromatography (hexane/ethyl acetate 25/1 v/v)