反应详情

温度

90 °C

A slurry of 2-(4-(1,3-dioxan-2-yl)-2-fluorophenyl)-6-chlorothiazolo[4,5-c]pyridine (1.00 g, 2.85 mmol), (Amphos)2PdCl2 (0.0505 g, 0.0713 mmol), potassium carbonate (1.34 g, 9.69 mmol), 1-phenylvinylboronic acid (0.928 g, 6.27 mmol) in 12 mL dioxane and 3 mL water was heated to 60° C. overnight in a sealed tube. Additional (Amphos)2PdCl2 (0.0505 g, 0.0713 mmol) was added and the temperature raised to 90° C. After 3 h, the homogeneous reaction mixture was cooled and treated with water and DCM. The organic layer was extracted with DCM, and combined organics were dried over sodium sulfate, filtered, and concentrated in vacuo. The solid was suspended in MTBE and filtered to give 2-(4-(1,3-dioxan-2-yl)-2-fluorophenyl)-6-(1-phenylvinyl)-thiazolo[4,5-c]pyridine as an off-white solid. MS (ESI) m/z: calculated: 418.1; Observed: 419.0 (M++1).

1. temperaturethe homogeneous reaction mixture was cooled
2. extractionThe organic layer was extracted with DCM
3. dry with materialcombined organics were dried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. filtrationfiltered