反应详情

温度

80 °C

A 5 L round bottom flask equipped with adapter, thermocouple and stir bar was charged with DMA (2.4 L) and degassed under vacuum and purged with N2 three times. Tetrakis was added to the mixture (35 g, 30.3 mmol) and the mixture was degassed under vacuum and purged with N2 three times. The reaction was heated to 80° C. for 30 min. 3-Fluoro-2-iodotoluene (230 g, 974 mmol) and zinc cyanide (68.7 g, 585 mmol) were added and the mixture was degassed under vacuum and purged with N2 three times. The mixture was heated to 80° C. for 16 hrs and allowed to cool to RT. The solution was added to 2.0 L aqueous solution of 1N NH4OH, which was then extracted three times with 1.5 L EtOAc, washed with 2 L brine, dried over Na2SO4, filtered, concentrated and purified by silica chromatography (PE/EA=10:1) to give the title compound.

1. customA 5 L round bottom flask equipped with adapter
2. customdegassed under vacuum
3. custompurged with N2 three times
4. customthe mixture was degassed under vacuum
5. custompurged with N2 three times
6. customthe mixture was degassed under vacuum
7. custompurged with N2 three times
8. temperatureThe mixture was heated to 80° C. for 16 hrs
9. temperatureto cool to RT
10. additionThe solution was added to 2.0 L aqueous solution of 1N NH4OH, which
11. extractionwas then extracted three times with 1.5 L EtOAc
12. washwashed with 2 L brine
13. dry with materialdried over Na2SO4
14. filtrationfiltered
15. concentrationconcentrated
16. custompurified by silica chromatography (PE/EA=10:1)