反应详情

3-hydroxy pyridine (97 mg, 1.02 mmol), 2-chloro-1-(4-(naphthalen-2-ylsulfonyl)piperazin-1-yl)ethanone (compound 5, 0.3 g, 0.85 mmol) and anhydrous potassium carbonate (0.352 g, 2.55 mmol) were stirred for over night in dry acetonitrile (20 mL). The mixture was poured into a large volume of water and the solution extracted with ether. Un-reacted phenol was removed with cold 1N NaOH solution. The ether extract was dried over anhydrous sodium sulphate, filtered and concentrated under reduced pressure. The crude material was purified by re-crystallization to yield the title compound (40 mg, 11.46% yield) as an off-white solid. 60% of the un-reacted starting material was also recovered from the reaction.

1. extractionthe solution extracted with ether
2. customUn-reacted phenol was removed with cold 1N NaOH solution
3. extractionThe ether extract
4. dry with materialwas dried over anhydrous sodium sulphate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe crude material was purified by re-crystallization