反应详情

5-(1H-Pyrazol-4-yl)-thiophene-3-carboxylic acid (0.075 g, 0.39 mmol) and 4,4-dimethylpiperidine hydrochloride (0.087 g, 0.58 mmol) were dissolved in DMF (3 mL) then DIPEA (0.2 g, 1.55 mmol) and HATU (0.175 g, 1.55 mmol) were added and the reaction mixture was stirred at room temperature overnight. The solvent was removed by evaporation then the residue was dissolved in DCM and washed with aqueous sodium hydrogen carbonate solution. The organics were dried by evaporation. The crude material was purified by HPLC, eluting with 5%-98% acetonitrile in water (0.1% formic acid) over 20 minutes. The fractions containing the desired product were freeze-dried to give the title compound (0.063 g). LCMS m/z 290.18 [M+H]+ R.T.=8.74 min (Analytical Method 2).

1. customThe solvent was removed by evaporation
2. dissolutionthe residue was dissolved in DCM
3. washwashed with aqueous sodium hydrogen carbonate solution
4. customThe organics were dried by evaporation
5. customThe crude material was purified by HPLC
6. washeluting with 5%-98% acetonitrile in water (0.1% formic acid) over 20 minutes
7. additionThe fractions containing the desired product
8. customwere freeze-dried