反应详情

温度

90 °C

1.02 g (4.0 mmol) of 1-(3-bromo-1,1-difluoropropyl)-4-fluorobenzene (precursor VC005) and 1.67 g (12.0 mmol) of K2CO3 were added to a solution of 620 mg (4.0 mmol) of 2-mercapto-nicotinic acid in DMF (10 ml), and the mixture was heated for 2 h at 90° C. Dilution with water (20 ml) was then carried out, and the pH was adjusted to −2 with 6M hydrochloric acid. Extraction with EA (3×40 ml) was then carried out. The combined organic phases were washed with water and brine, dried over Na2SO4, filtered and concentrated in vacuo. CC (hexane/EA 1:4) of the residue yielded 400 mg (1.2 mmol, 31%) of 2-(3,3-difluoro-3-(4-fluorophenyl)propylthio)-nicotinic acid.

1. extractionExtraction with EA (3×40 ml)
2. washThe combined organic phases were washed with water and brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo