反应详情

温度

90 °C

A mixture of 2-{[2-bromo-4-(trifluoromethyl)phenyl]sulfonyl}-1,3,4,10b-tetrahydropyrido[4′,3′:3,4]pyrrolo[1,2-a]pyrazin-6(2H)-one (250 mg), trimethylboroxin (0.190 mL), potassium carbonate (189 mg) and Pd(PPh3)4 (103 mg) was heated to 90° C. under argon for 18 hours. The reaction mixture was partitioned between EtOAc and aqueous saturated sodium bicarbonate solution. The aqueous phase was re-extracted with EtOAc. The combined organic phases were washed with brine, dried through a hydrophobic frit and evaporated to a brown oil. This was purified by chromatography eluting with 0-5% methanol in DCM over 12 column volumes. The clean fractions were combined and evaporated to a pale yellow gum. This was purified further to remove triphenylphosphine oxide by MDAP. The clean fraction was evaporated to give the title compound as a white solid (46 mg).

1. customThe reaction mixture was partitioned between EtOAc and aqueous saturated sodium bicarbonate solution
2. extractionThe aqueous phase was re-extracted with EtOAc
3. washThe combined organic phases were washed with brine
4. customdried through a hydrophobic frit
5. customevaporated to a brown oil
6. customThis was purified by chromatography
7. washeluting with 0-5% methanol in DCM over 12 column volumes
8. customevaporated to a pale yellow gum
9. customThis was purified further
10. customto remove triphenylphosphine oxide by MDAP
11. customThe clean fraction was evaporated