反应详情

Potassium carbonate (61 mg, 0.229 mmol) was added to a solution of 5-chloro-6-(3,3,3-trifluoropropoxy)pyridin-3-ol (Preparation 67, 45 mg, 0.19 mmol) in DMSO (2 mL) and the reaction mixture was stirred under a nitrogen atmosphere at room temperature for 5 minutes. 4-(Bromomethyl)-2,5-difluoro-N-(methylsulfonyl)benzamide (Preparation 10, 63 mg, 0.19 mmol) was then added and the resulting mixture stirred under nitrogen at room temperature for 120 hours. The reaction mixture was diluted with aqueous hydrochloric acid solution (2 M, 15 mL), extracted with EtOAc (20 mL). The organic layer was washed with aqueous hydrochloric acid solution (2 M, 2×10 mL), dried over magnesium sulfate, filtered and evaporated in vacuo. The resulting crude solid was triturated with TBME/heptane (2:1), washed with heptane and dried in vacuo to yield the title compound as an off-white solid (73 mg, 74%):

1. stirringthe resulting mixture stirred under nitrogen at room temperature for 120 hours
2. extractionextracted with EtOAc (20 mL)
3. washThe organic layer was washed with aqueous hydrochloric acid solution (2 M, 2×10 mL)
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. customevaporated in vacuo
7. customThe resulting crude solid was triturated with TBME/heptane (2:1)
8. washwashed with heptane
9. customdried in vacuo