反应详情

In reactor bottle under N2 were combined fine cesium carbonate (0.209 g, 0.644 mmol) and diethyl malonate (0.195 mL, 1.29 mmol) in DMF (3 mL). The resulting slurry was allowed to stir for 1 h at ambient temperature. To the mixture was added 2-(2-fluoro-4-vinylphenyl)-5-(1-phenylcyclopropyl)thiazolo[5,4-b]pyridine (0.200 g, 0.537 mmol) and the reaction mixture was heated to 35° C. for 1.5 h. The reaction mixture was cooled to 0° C. and acidified using 1 N aq. HCl, extracted with EtOAc, and the organic layer was dried over MgSO4, filtered, and concentrated in vacuo. Purification by silica gel chromatography provided diethyl 2-(3-fluoro-4-(5-(1-phenylcyclopropyl)thiazolo[5,4-b]pyridin-2-yl)phenethyl)malonate. MS (ESI) m/z: calculated: 532.2; Observed: 533.1 (M++1).

1. customIn reactor bottle under N2 were combined fine
2. temperaturethe reaction mixture was heated to 35° C. for 1.5 h
3. temperatureThe reaction mixture was cooled to 0° C.
4. extractionextracted with EtOAc
5. dry with materialthe organic layer was dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customPurification by silica gel chromatography