反应详情

A mixture in DMF (1 ml) of trans-4-[2-(4-thieno[2,3-c]pyridin-7-yl-piperazin-1-yl)-ethyl]-cyclohexylamine trihydrochloride (intermediate A; 90 mg, 0.20 mmol), propionic acid (15 mg, 0.20), iPr2NEt (103 mg, 0.80 mmol) and TBTU (67 mg, 0.21 mmol) was stirred 18 h at room temperature. Sat. aq. NaHCO3 sol. was added and the product was extracted with EtOAc (3×). The organic layers were washed with water and brine, dried (MgSO4) and the solvent was evaporated. The crude product was purified by flash chromatography on silica gel (CH2Cl2/MeOH 95:5) to yield the title compound as an off-white crystalline solid (66 mg, 83%), MS (ISP) m/z=401.3 [(M+H)+].

1. extractionthe product was extracted with EtOAc (3×)
2. washThe organic layers were washed with water and brine
3. dry with materialdried (MgSO4)
4. customthe solvent was evaporated
5. customThe crude product was purified by flash chromatography on silica gel (CH2Cl2/MeOH 95:5)