反应详情

A mixture of methyl 2-bromo-3-methylbenzoate (22.33 g, 97.5 mmol), potassium phosphate (82.8 g, 390 mmol), [1,1′-bis(diphenylphosphino)-ferrocene]dichloro palladium (II), complex with dichloromethane (1:1) (3.98 g, 4.87 mmol), and p-trifluoromethylphenylboronic acid (22.2 g, 117 mmol) in 500 mL of DME is degassed and refluxed under an atmosphere of argon overnight. The mixture is concentrated, poured into water and extracted with ethyl acetate. The combined organic extracts are washed with brine, dried over magnesium sulphate, filtered and evaporated under reduced pressure. The residue is purified by silica gel chromatography eluting with ethyl acetate/toluene (1:9) to give methyl 6-methyl-4′-trifluoromethyl-biphenyl-2-carboxylate.

1. customis degassed
2. temperaturerefluxed under an atmosphere of argon overnight
3. concentrationThe mixture is concentrated
4. additionpoured into water
5. extractionextracted with ethyl acetate
6. washThe combined organic extracts are washed with brine
7. dry with materialdried over magnesium sulphate
8. filtrationfiltered
9. customevaporated under reduced pressure
10. customThe residue is purified by silica gel chromatography
11. washeluting with ethyl acetate/toluene (1:9)