反应详情

To a solution of 2-(4-chloro-2,6-dimethyl-phenoxy)-4-(1-ethyl-2-hydroxy-propylamino)-6-methyl-nicotinic acid methyl ester (50 mg, 0.123 mmol) in dry THF was added NaH and stirred for 20 min. An excess of Mel was added and the resulting mixture was stirred at rt overnight. The mixture cooled to rt and quenched with water and extracted with ethyl acetate. The organic layer was separated, washed with water, dried over anhydrous sodium sulfate, filtered, and concentrated to dryness to give an oil. The oil was purified through silica gel column chromatography using 20% ethyl acetate in hexane as an eluent to give the title compound as a clear oil. 1H NMR(CDCl3) d 8.20(d, 1H), 7.00(s, 2H), 6.14&6.10(two sets of s, 1H), 3.859s, 3H), 3.47(m, 1H), 3.39&3.37(two set of s, 3H), 2.08(s, 3H), 2.06(s, 6H), 1.75(m, 1H), 1.58(m, 1H), 1.14(t, 3H), 0.95(t, 3H) ppm.

1. additionAn excess of Mel was added
2. stirringthe resulting mixture was stirred at rt overnight
3. customquenched with water
4. extractionextracted with ethyl acetate
5. customThe organic layer was separated
6. washwashed with water
7. dry with materialdried over anhydrous sodium sulfate
8. filtrationfiltered
9. concentrationconcentrated to dryness
10. customto give an oil
11. customThe oil was purified through silica gel column chromatography