反应详情

温度

140 °C

To a microwave vial was added 8-Bromo-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulene-2-carboxylic acid (2-hydroxyethyl)-isopropylamide (0.100 grams, 0.243 mmol) in 2M sodium carbonate (0.500 mL) and ACN (0.636 mL), and then 4-(2-(5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-2-yl)ethyl)morpholine (0.292 mmol) was added. This solution was degassed by bubbling nitrogen through the solution for several minutes. Finally, palladium tetrakis(triphenylphosphine)palladium(0) was added and the vial was tightly capped. The reaction mixture was then flash heated on a Biotage microwave at 140° C. for 20 minutes. The cooled reaction mixture was diluted with EtOAc and the organic was washed with water, then saline and dried (Na2SO4) before concentration to a solid. The crude material was purified by preparative RP-HPLC to give 267. MS: (ESI+)=495.1

1. customThis solution was degassed
2. customby bubbling nitrogen through the solution for several minutes
3. additionFinally, palladium tetrakis(triphenylphosphine)palladium(0) was added
4. customthe vial was tightly capped
5. customThe cooled reaction mixture
6. washthe organic was washed with water
7. dry with materialsaline and dried (Na2SO4)
8. concentrationbefore concentration to a solid
9. customThe crude material was purified by preparative RP-HPLC