Hydrochloric Acid → HCID 14052568, compound

A mixture of 3-bromo-2,5,6-trifluorotoluene (11.0 g) and cupric cyanide (5.3 g) in N-methylpyrrolidone (15 ml) was stirred at 150° to 160° C. in a sealed tube for 4.5 hours. After cooling, to the reacting mixture was added a solution of ferric chloride (20 g) and concentrated hydrochloric acid (5 ml) in water (30 ml) and stirred at 50° to 60° C. for 20 minutes. The reacting mixture was extracted with ether, the organic layer was washed with aqueous hydrochloric acid solution, water and saturated aqueous sodium chloride solution successively, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give the title compound (7.83 g) as pale brown oil.

1. temperatureAfter cooling, to the reacting mixture
2. stirringstirred at 50° to 60° C. for 20 minutes
3. extractionThe reacting mixture was extracted with ether
4. washthe organic layer was washed with aqueous hydrochloric acid solution, water and saturated aqueous sodium chloride solution successively
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated under reduced pressure

ORD record

ord-3400fbc7f7404634af49de6bfc2a5e4a

Source dataset

uspto-grants-1990_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04894458