反应详情

4,4-Difluoro-azepane trifluoroacetate (Synthesis 47, 0.113 g, 0.45 mmol) was dissolved in THF (1 mL) and added to 5-oxazol-4-yl-thiophene-3-carboxylic acid (0.059 g, 0.30 mmol). DIPEA (0.154 mL, 0.90 mmol) was added followed by HATU (0.125 g, 0.33 mmol) and the reaction mixture was then stirred at room temperature overnight. The mixture was diluted with DCM then washed with aqueous sodium carbonate solution. The organics were dried over sodium sulfate, filtered and evaporated. The crude material was purified by HPLC, eluting with 5%-98% methanol in water (0.1% formic acid). The fractions containing the desired product were freeze-dried to give the title compound (0.029 g). LCMS m/z 313.15 [M+H]+ R.T.=8.31 min (Analytical Method 10).

1. washthen washed with aqueous sodium carbonate solution
2. dry with materialThe organics were dried over sodium sulfate
3. filtrationfiltered
4. customevaporated
5. customThe crude material was purified by HPLC
6. washeluting with 5%-98% methanol in water (0.1% formic acid)
7. additionThe fractions containing the desired product
8. customwere freeze-dried