反应详情

In a nitrogen atmosphere, to 53 mL of a 1M tetrahydrofuran solution of 1-trifluoromethylethenyl zinc bromide prepared according to a method described in the literatures, 7.1 g of 2-chloro-5-iodobenzotrifluoride and 0.65 g of dichlorobis(triphenylphosphine) palladium (II) were added and the resultant mixture was stirred while heating the mixture to reflux for 2.5 hours. After the completion of the reaction, the reaction mixture was left to be cooled down to room temperature and 200 mL of hexane was added to the reaction mixture, followed by filtering off the deposited insoluble substance. The resultant filtrate was washed with water (50 mL×1) and then dehydrated and dried over saturated saline and anhydrous sodium sulfate in this order and the solvent was distilled off under reduced pressure. The resultant residue was purified by silica gel column chromatography eluting with hexane to obtain 4.8 g of the objective substance as a colorless oily substance.

1. additionwere added
2. temperaturewhile heating the mixture
3. temperatureto reflux for 2.5 hours
4. customAfter the completion of the reaction
5. waitthe reaction mixture was left
6. filtrationby filtering off the deposited insoluble substance
7. washThe resultant filtrate was washed with water (50 mL×1)
8. dry with materialdried over saturated saline and anhydrous sodium sulfate in this order
9. distillationthe solvent was distilled off under reduced pressure
10. customThe resultant residue was purified by silica gel column chromatography
11. washeluting with hexane
12. customto obtain 4.8 g of the objective substance as a colorless oily substance