反应详情

Under argon, a solution of 1.29 g (7.02 mmol) of (+/−)-ethyl 4,4,4-trifluoro-3-methylbutanoate in 2 ml of abs. toluene was added dropwise to 8.1 ml of a 1 M solution, cooled to −10° C., of lithium hexamethyldisilazide in toluene (8.1 mmol). After 10 min at −10° C., a mixture of 1.0 g (5.4 mmol) of 1-bromo-4-ethylbenzene, 36.4 mg (0.16 mmol) of palladium(II) acetate and 134 mg (0.34 mmol) of 2-dicyclohexylphosphino-2′-(N,N-dimethylamino)biphenyl in 5 ml of abs. toluene was added to this reaction mixture. After the addition had ended, the mixture was warmed to RT and then stirred first at RT for 1 h and then at 80° C. for a further 3 h. After cooling to RT, the precipitated salts were filtered off with suction, the residue was washed with toluene and the combined filtrates were concentrated under reduced pressure. This gave 1.26 g of crude product (80.9% of theory) which was reacted as such.

1. additionAfter the addition
2. waitat 80° C. for a further 3 h
3. temperatureAfter cooling to RT
4. filtrationthe precipitated salts were filtered off with suction
5. washthe residue was washed with toluene
6. concentrationthe combined filtrates were concentrated under reduced pressure
7. customThis gave 1.26 g of crude product (80.9% of theory) which was reacted as such