反应详情

温度

120 °C

Ethyl 1-(4-bromothiazol-2-yl)-4-ethyl-piperidine-4-carboxylate (56 mg, 0.16 mmol), 2-(ethylcarbamoylamino)-7-(2-pyridyl)-1,3-benzothiazol-5-yl-boronic acid (50 mg, 0.15 mmol), and cesium carbonate (42 mg, 0.22 mmol) were suspended in DMF (1 mL) in a 5 mL microwave vessel. The resulting mixture was degassed with Ar for 5 min. [1,1′-Bis(diphenylphosphino)ferrocene]dichloropalladium(II), complex with dichloromethane (10 mg, 0.01 mmol), was added to the mixture, then the vessel sealed and heated at 120° C. for 60 min in a microwave. The mixture was cooled to rt then evaporated to dryness and the crude residue purified over a 12 g silica-gel column using a MeOH: DCM elution gradient (0-5%) to obtain the product as a viscous oil (30 mg, 36% yield). MS: 565.13 [M+H]+.

1. additionwas added to the mixture
2. customthe vessel sealed
3. temperatureThe mixture was cooled to rt
4. customthen evaporated to dryness
5. customthe crude residue purified over a 12 g silica-gel column
6. washDCM elution gradient (0-5%)