反应详情

温度

150 °C

A microwave tube equipped with a magnetic stirrer was charged with 167e (301 mg, 1.47 mmol), 2,6-dibromobenzyl acetate 104g (1.1 g, 3.0 mmol), CuI (140 mg, 0.7 mmol) Cs2CO3 (961 mg, 3.0 mmol), N′,N′,N′,N′-tetramethylethylenediamine (0.22 mL, 1.5 mmol) and 1,2-dimethoxyethane (4.1 mL). The mixture was heated in microwave to 150° C. for 3 h. After this time, the mixture was filtered and the resulting solid was washed with 9:1 CH2Cl2/MeOH (50 mL). The combined organics were washed with brine (20 mL), dried over sodium sulfate, filtered and concentrated under reduced pressure. The resulting residue was purified by column chromatography eluting with a gradient of hexanes-ethyl acetate to afford a 32% yield (200 mg) of 167f.

1. customA microwave tube equipped with a magnetic stirrer
2. filtrationAfter this time, the mixture was filtered
3. washthe resulting solid was washed with 9:1 CH2Cl2/MeOH (50 mL)
4. washThe combined organics were washed with brine (20 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 hexanes-ethyl acetate