反应详情

2-[2-(3-Trifluoromethyl-4,5,6,7-tetrahydroindazol-1-yl)-acetylamino]-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxylic acid (20 mg, 0.047 mmol) was dissolved in a solution of DCM (800 μL) and DMF (200 μL). Polymer supported carbodiimide (loading 1.22 mmol/g, 53 mg, 0.064 mmol) was added, followed by ethylamine (2.0 M solution in THF, 94.0 μl, 0.188 mmol). The resultant mixture was heated in a Biotage SmithCreator microwave at 120° C. for 15 min. The resin was filtered off and washed through with MeOH (2×50 mL), EtOAc (2×20 mL) and MeCN (2×20 mL). The combined filtrate was concentrated in vacuo, and the residue obtained purified by preparative reverse phase HPLC to afford the title compound as a white solid (1 mg, 0.003 mmol, 6%).

1. additionwas added
2. filtrationThe resin was filtered off
3. washwashed through with MeOH (2×50 mL), EtOAc (2×20 mL) and MeCN (2×20 mL)
4. concentrationThe combined filtrate was concentrated in vacuo
5. customthe residue obtained
6. custompurified by preparative reverse phase HPLC