反应详情

3-(trifluoromethyl)-4,5,6,7-tetrahydroindazole (50 mg, 0.263 mmol) was dissolved in DMF (2 mL). NaH (60% [w/w] suspension in oil, 11 mg, 0.275 mmol) was added followed by potassium iodide (2 mg, catalyst) and the reaction mixture stirred at RT for 30 min. 2-(3-chloropropanamido)-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxamide (75 mg, 0.262 mmol) was then added and the reaction mixture heated at 120° C. for 400 sec in a Biotage SmithCreator microwave. Water was added followed by EtOAc (3×10 mL) extraction. The EtOAc layers were washed with water (5×5 mL), brine, dried over MgSO4, filtered and the solvent removed in vacuo to give a yellow gum. Purification by preparative reverse phase HPLC gave desired product (22.7 mg, 0.052 mmol, 20%).

1. temperaturethe reaction mixture heated at 120° C. for 400 sec in a Biotage SmithCreator microwave
2. extractionfollowed by EtOAc (3×10 mL) extraction
3. washThe EtOAc layers were washed with water (5×5 mL), brine
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. customthe solvent removed in vacuo
7. customto give a yellow gum
8. customPurification by preparative reverse phase HPLC