反应详情

温度

90 °C

Cs2CO3 (0.495 g, 1.52 mmol) was added to a solution of (3R)-(7-chloro-thieno[3,2-b]pyridin-2-yl)-(3-methoxy-pyrrolidin-1-yl)-methanone (0.228 g, 0.76 mmol) and 2-methyl-1H-indol-5-ol (0.223 9, 1.52 mmol) in DMF (5 mL), and the resulting solution was heated to 90° C. After 20 h the reaction was quenched with water, EtOAc was added, and the layers were separated. The aqueous layer was extracted with EtOAc, and the combined organic layers were dried over Na2SO4 then concentrated. The resulting material was purified on silica gel by flash column chromatography, eluting with CH2Cl2/MeOH (98/2) to afford the title compound as a white solid (0.26 g, 84%). MS: 408.8 (MH+); HPLC Rf: 5.394 min.; HPLC purity: 97%.

1. customAfter 20 h the reaction was quenched with water, EtOAc
2. additionwas added
3. customthe layers were separated
4. extractionThe aqueous layer was extracted with EtOAc
5. dry with materialthe combined organic layers were dried over Na2SO4
6. concentrationthen concentrated
7. customThe resulting material was purified on silica gel by flash column chromatography
8. washeluting with CH2Cl2/MeOH (98/2)