反应详情

A solution of 0.34 cm3 (4.66 mmol) of thionyl chloride and 0.555 g (4.66 mmol) of benzotriazole in 40 cm3 of dichloromethane is added at a temperature in the region of 20° C. under an argon atmosphere to 0.646 g (3.8 mmol) of 2,5-difluorocinnamyl alcohol in solution in 40 cm3 of dichloromethane. After stirring for 10 minutes, the reaction mixture is filtered on No. 3 sintered glass and the solid residue rinsed with twice 10 cm3 of dichloromethane. The filtrate is washed 3 times with 30 cm3 of water. The organic phase is dried over magnesium sulfate and filtered to give a solution of 2-[(1E)-3-chloro-1-propenyl]-1,4-difluorobenzene (3.8 mmol) which is then concentrated to dryness under reduced pressure (2.7 kPa) at a temperature in the region of 20° C., before dissolution in acetonitrile.

1. filtrationthe reaction mixture is filtered on No
2. wash3 sintered glass and the solid residue rinsed with twice 10 cm3 of dichloromethane
3. washThe filtrate is washed 3 times with 30 cm3 of water
4. dry with materialThe organic phase is dried over magnesium sulfate
5. filtrationfiltered