反应详情

A solution of 3-{[2-fluoro-1-(fluoromethyl)ethyl]oxy}-5-hydroxy-N-(1-methyl-1H-pyrazol-3-yl)benzamide (100 mg, 0.32 mmol), N-(2-{[(1,1-dimethylethyl)(dimethyl)silyl]oxy}ethyl)-2,3,4-trifluoro-N-methylbenzamide (112 mg, 0.32 mmol) and potassium carbonate (89 mg, 0.64 mmol) in DMA (2 mL) was heated in a microwave reactor for 2 hours. Water (20 mL) was added and the solution extracted with ethyl acetate. The ethyl acetate layer was washed with brine (20 mL), dried (MgSO4) and evaporated to a residue which was taken up in DCM (10 mL) and TFA (5 drops) added. The mixture was stirred at RT for 2 hours. The solvent was evaporated to a residue, which was chromatographed by preparative HPLC on C18 reversed phase, eluting with 5-95% acetonitrile (+0.2% TFA) in water (+0.2% TFA), to give the required product (5 mg).

1. extractionthe solution extracted with ethyl acetate
2. washThe ethyl acetate layer was washed with brine (20 mL)
3. dry with materialdried (MgSO4)
4. customevaporated to a residue which
5. additionTFA (5 drops) added
6. customThe solvent was evaporated to a residue, which
7. customwas chromatographed by preparative HPLC on C18 reversed phase
8. washeluting with 5-95% acetonitrile (+0.2% TFA) in water (+0.2% TFA)