反应详情

To 1H-Pyrrolo[2,3-b]pyridine-5-carbonitrile (632, 3.00 g, 0.0210 mol) in isopropyl alcohol (120 mL) were added dimethylamine hydrochloride (1.91 g, 0.0235 mol) and formaldehyde (0.708 g, 0.0236 mol). The reaction was heated to reflux overnight, then concentrated, poured into water, and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated and purified by silica gel column chromatography eluting with 5% to 30% methanol in dichloromethane containing 0.3% triethyl amine to give the desired compound (633, 2.0 g, 48%).

1. temperatureThe reaction was heated
2. temperatureto reflux overnight
3. concentrationconcentrated
4. additionpoured into water
5. extractionextracted with ethyl acetate
6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
7. filtrationfiltered
8. concentrationThe filtrate was concentrated
9. custompurified by silica gel column chromatography
10. washeluting with 5% to 30% methanol in dichloromethane containing 0.3% triethyl amine