反应详情

温度

130 °C

A microwave tube equipped with a magnetic stirrer was charged with 285c (190 mg, 0.5 mmol), 230a (350 mg, 0.7 mmol), 1,2-dimethoxyethane (6.4 mL) and 1M aqueous sodium carbonate (1.6 mL). After bubbling N2 for 15 min, Pd(PPh3)4 (31 mg, 0.03 mmol) was added. The mixture was heated in microwave to 130° C. for 15 min. After this time, ethyl acetate (5 mL) and water (5 mL) were added. The separated aqueous layer was extracted with ethyl acetate (2×5 mL). The combined organics were washed with brine (10 mL), dried over sodium sulfate, filtered and concentrated under reduced pressure. The resulting residue was purified by column chromatography eluting with a gradient of methylene chloride-60:35:5 methylene chloride:diethyl ether:methanol to afford a 35% yield (120 mg) of 285d.

1. customA microwave tube equipped with a magnetic stirrer
2. customAfter bubbling N2 for 15 min
3. extractionThe separated aqueous layer was extracted with ethyl acetate (2×5 mL)
4. washThe combined organics were washed with brine (10 mL)
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe resulting residue was purified by column chromatography
9. washeluting with a gradient of methylene chloride-60:35:5 methylene chloride