反应详情

温度

80 °C

To 6-fluoro-3-(3-fluorophenyl)-2-methyl-benzoic acid (3 g, 12.0 mmol, 1 eq) was added SOCl2 (60 mL) and the reaction heated at 80° C. overnight. The resulting mixture was concentrated in vacuo and the residue that remained dissolved in THF (20 mL) and added dropwise to a mixture of 3-amino-2,4-difluoro-phenol (1.93 g, 13.2 mmol, 1.1 eq) and NaHCO3 (2.32 g, 36.2 mmol, 3 eq) in THF (5 mL). After the addition, the reaction mixture was stirred at room temperature for 30 min. Water was added and the aqueous layer was extracted with EtOAc. The combined organic extracts were dried (Na2SO4), filtered and evaporated in vacuo to give the title compound (500 mg, 11%) which was used without further purification.

1. concentrationThe resulting mixture was concentrated in vacuo
2. dissolutionthe residue that remained dissolved in THF (20 mL)
3. additionAfter the addition
4. extractionthe aqueous layer was extracted with EtOAc
5. dry with materialThe combined organic extracts were dried (Na2SO4)
6. filtrationfiltered
7. customevaporated in vacuo