反应详情

Combine 2-(4-methoxy-phenyl)-5,6-dihydro-4H-thieno[2,3-c]pyridin-7-one (0.234 g, 0.90 mmol), 1-[2-(4-bromo-2-methoxy-phenoxy)-ethyl]-pyrrolidine (Bastian, J. A., et al WO 9725033 A1) (0.271 g, 0.90 mmol), N,N′-dimethyl-ethane-1,2-diamine (16 mg, 0.18 mmol), K2CO3 (0.249 g, 1.81 mmol), and CuI (17 mmol, 0.09 mmol) in toluene (10 mL) and stir at 110° C. for 48 h. Dilute with EtOAc (100 mL) and wash with water (50 mL), containing NH3—H2O (5 mL) three times. Dry over Na2SO4, filter and purify the material by chromatography, eluting with 7% 2 M NH3 in CH3OH, and 93% CH2Cl2 to give 0.125 g. Dissolve the material in CH3OH (5 mL) and treat with 1.0 M HCl in EtOH (270 μL, 0.27 mmol). Stir at RT for 5 min and concentrate to give the title compound (0.133 g, 0.26 mmol, 100%). LC-MS/ES m/z 479.3 [M+H]+.

1. washwash with water (50 mL)
2. additioncontaining NH3—H2O (5 mL) three times
3. dry with materialDry over Na2SO4
4. filtrationfilter
5. custompurify the material by chromatography
6. washeluting with 7% 2 M NH3 in CH3OH, and 93% CH2Cl2
7. customto give 0.125 g
8. concentrationconcentrate