反应详情

To a solution of 2,6-difluoro-3-triisopropylsilyloxy-benzoic acid (see example 2) (7 g, 21.1 mmol, 1.0 eq) in MeOH (100 mL) was added SOCl2 (10 mL) dropwise. The reaction mixture was heated at reflux for 3 h, then cooled and the solvent removed in vacuo. Water was added and the aqueous layer was extracted with EtOAc. The organic extract was washed with water and brine, dried (Na2SO4), filtered and evaporated in vacuo to give the title compound as a solid (3 g, 75%) which was used in the next step without further purification.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 3 h
3. temperaturecooled
4. customthe solvent removed in vacuo
5. additionWater was added
6. extractionthe aqueous layer was extracted with EtOAc
7. extractionThe organic extract
8. washwas washed with water and brine
9. dry with materialdried (Na2SO4)
10. filtrationfiltered
11. customevaporated in vacuo