反应详情

A solution of 2-Methoxy-8-trimethylsilanylethynyl-[1,5] naphthyridine in methanol (80 mL) was treated with potassium carbonate (4.49 g, 32 mmole) and stirred 1.5 hrs. The reaction mixture was concentrated to dryness, redissolved in ethyl acetate, and partitioned with brine. The biphasic mixture was filtered to facilitate separation. Organic layer was dried over sodium sulfate, filtered, concentrated and chromatographed in 1:1 ethyl acetate:hexane to give the product as a cream colored solid. δH (CDCl3, 400 MHz), 8.73 (d, J=4Hz, 1 H), 8.20 (d, J=9 Hz, 1 H), 7.68 (d, J=4 Hz, 1H), 7.16 (d, J=9 Hz, 1 H), 4.15 (s, 3H), 3.67 (s, 1H).

1. concentrationThe reaction mixture was concentrated to dryness
2. dissolutionredissolved in ethyl acetate
3. custompartitioned with brine
4. filtrationThe biphasic mixture was filtered
5. customseparation
6. dry with materialOrganic layer was dried over sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated
9. customchromatographed in 1:1 ethyl acetate
10. customhexane to give the product as a cream