反应详情

温度

100 °C

In a nitrogen atmosphere, to 19 mL of a 1M tetrahydrofuran solution of 1-trifluoromethylethenyl zinc bromide prepared according to a method described in the literatures, a solution of 2.2 g of 5-bromo-2,3-dichlorotoluene in 10 mL of N,N-dimethylformamide was added and tetrahydrofuran was distilled off under reduced pressure. To the remaining N,N-dimethylformamide solution, 0.26 g of dichlorobis(triphenylphosphine) palladium (II) was added and the resultant mixture was stirred at 100° C. for 3.5 hours. After the completion of the reaction, the reaction mixture was left to be cooled down to room temperature and 200 mL of a tetrahydrofuran-hexane (2:5) mixture was added to the reaction mixture, followed by filtering off the deposited insoluble substance. The resultant filtrate was washed with water (100 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 2.3 g of the objective substance as a brown oily substance.

1. distillationtetrahydrofuran was distilled off under reduced pressure
2. additionTo the remaining N,N-dimethylformamide solution, 0.26 g of dichlorobis(triphenylphosphine) palladium (II) was added
3. customAfter the completion of the reaction
4. waitthe reaction mixture was left
5. temperatureto be cooled down to room temperature
6. filtrationby filtering off the deposited insoluble substance
7. washThe resultant filtrate was washed with water (100 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 2.3 g of the objective substance as a brown oily substance