反应详情

温度

110 °C

Dissolve 2-(thieno[3,2-b]pyridin-7-yl)malonic acid diethyl ester (12.90 g, 44.0 mmol) in dimethyl sulfoxide (295 mL). Add water (0.79 mL) and lithium chloride (3.73 g, 87.9). Heat the solution to 110° C. for 3 hours. Quench the reaction with saturated brine (3 L) and extract with ethyl acetate (3×1 L). Rewash the organic layers with saturated brine (1 L). Treat the organic layers with magnesium sulfate, filter and concentrate. The residue was purified on silica using 25% ethyl acetate/hexanes to yield the desired compound (5.25 g, 54%).

1. customQuench
2. customthe reaction with saturated brine (3 L)
3. extractionextract with ethyl acetate (3×1 L)
4. additionTreat the organic layers with magnesium sulfate
5. filtrationfilter
6. concentrationconcentrate
7. customThe residue was purified on silica using 25% ethyl acetate/hexanes