反应详情

Into 5 ml of dry dimethylformamide containing 150 mg of sodium hydride (60% suspension in mineral oil) was added 292 mg of 2-hydroxypyridine. After stirring the mixture at room temperature for 15 minutes, 1.2 g of ethyl 6-[p-(5-bromopentyloxy)phenoxy]-2,2-dimethylhexanoate was added thereto. The mixture was stirred at room temperature for 12 hours, and thereafter the solvent was removed from the reaction solution under reduced pressure. The remaining oily substance was dissolved in chloroform, washed with water, and then dried over anhydrous magnesium sulfate. After drying, the solvent was distilled off under reduced pressure. The remaining oily substance was subjected to silica gel column chromatography and the product was eluted out using as an eluent chloroform-methanol (99:1). The solvent was distilled off from the eluate under reduced pressure to give the desired ethyl 6-[p-[5-(2-pyridyloxy)pentyloxy)phenoxy]-2,2-dimethylhexanoate as an oily substance (495 mg).

1. stirringThe mixture was stirred at room temperature for 12 hours
2. customthe solvent was removed from the reaction solution under reduced pressure
3. dissolutionThe remaining oily substance was dissolved in chloroform
4. washwashed with water
5. dry with materialdried over anhydrous magnesium sulfate
6. customAfter drying
7. distillationthe solvent was distilled off under reduced pressure
8. washthe product was eluted out
9. distillationThe solvent was distilled off from the eluate under reduced pressure