反应详情

温度

120 °C

NaH (60% [w/w] suspension in oil, 10 mg, 0.25 mmol) was added to a solution of ethyl-3-(trifluoromethyl)pyrazole-4-carboxylate (25 mg, 0.056 mmol) in DMF (2 mL). The reaction mixture was stirred at RT for 60 min before the addition of 2-(2-bromoacetamido)-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxamide. The reaction mixture was heated at 120° C. for 10 min in the microwave. Water (5 μL) was added and the reaction mixture extracted with EtOAc (3×10 mL). The combined EtOAc layers were washed with water (5×5 mL), brine (5 mL), dried over MgSO4, filtered and the solvent removed under reduced pressure to give the crude reaction mixture as a yellow solid (44 mg, 0.01 mmol). Purification by preparative reverse phase HPLC gave the desired product (10 mg, 0.024 mmol, 19%).

1. extractionthe reaction mixture extracted with EtOAc (3×10 mL)
2. washThe combined EtOAc layers were washed with water (5×5 mL), brine (5 mL)
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. customthe solvent removed under reduced pressure
6. customto give the crude
7. customPurification by preparative reverse phase HPLC