反应详情

Into a cooled solution (−78° C.) of 2-fluoro-4-vinylbenzonitrile (1.3 g, 8.8 mmol; see step (i) above) in 40 mL of CH2Cl2 and 5 mL of methanol was bubbled ozone (50 L/h, 29 g/m3) for 30 min. Argon was subsequently bubbled through to remove excess ozone. Sodium borohydride (0.67 g, 0.018 mol) was added and the cooling bath was removed. The mixture was stirred and allowed to react for 1 h. The mixture was evaporated and 2M HCl was added. The mixture was extracted twice with diethyl ether and the combined ether fraction was dried (Na2SO4) and evaporated. The crude product crystallised. Yield: 1.1 g (81%).

1. customArgon was subsequently bubbled through
2. customto remove excess ozone
3. customthe cooling bath was removed
4. customto react for 1 h
5. customThe mixture was evaporated
6. addition2M HCl was added
7. extractionThe mixture was extracted twice with diethyl ether
8. dry with materialthe combined ether fraction was dried (Na2SO4)
9. customevaporated
10. customThe crude product crystallised