反应详情

温度

110 °C

To a 20 mL microwave tube was added a stir bar, 3-bromo-6-methoxy-2-methylbenzonitrile (4.0 g, 18 mmol), vinyl ethoxy tributyltin (9.5 g, 26 mmol), palladium tetrakis (1.0 g, 0.88 mmol), and anhydrous toluene (15 mL). The tube was capped, degassed and purged with N2. The reaction mixture was heated to 110° C. for 12 hours. The tube was cooled to room temperature and treated with 4 M HCl (10 mL) and stirred for 1 hour. The crude product was extracted with EtOAc. The extraction was washed with brine, dried with Na2SO4, filtered and concentrated in vacuo. The crude residue was purified by silica gel column chromatography (Hexanes:EtOAc=1:1) to afford the title product.

1. additionTo a 20 mL microwave tube was added a stir bar
2. customThe tube was capped
3. customdegassed
4. custompurged with N2
5. temperatureThe tube was cooled to room temperature
6. additiontreated with 4 M HCl (10 mL)
7. extractionThe crude product was extracted with EtOAc
8. extractionThe extraction
9. washwas washed with brine
10. dry with materialdried with Na2SO4
11. filtrationfiltered
12. concentrationconcentrated in vacuo
13. customThe crude residue was purified by silica gel column chromatography (Hexanes:EtOAc=1:1)