反应详情

温度

200 °C

2-[2-(3-Trifluoromethyl-4,5,6,7-tetrahydroindazol-1-yl)-acetylamino]-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxylic acid (200 mg, 0.47 mmol) and copper powder (45 mg, 0.70 mmol) were suspended in quinoline (4 mL) and the resulting mixture heated in a Biotage SmithCreator microwave at 200° C. for 10 min. The mixture was diluted with water (5 mL), acidified to pH 1 with 5 M HCl, and extracted with diethyl ether (3×50 mL). The combined organics were dried over sodium sulfate and concentrated in vacuo. The residue obtained was purified by silica gel chromatography using DCM as eluent, to afford the title compound as an off-white solid (170 mg, 0.44 mmol, 95%).

1. extractionextracted with diethyl ether (3×50 mL)
2. dry with materialThe combined organics were dried over sodium sulfate
3. concentrationconcentrated in vacuo
4. customThe residue obtained
5. customwas purified by silica gel chromatography