反应详情

温度

120 °C

To a degassed solution of N-allyl-3-chloro-N-[(1R)-2,3-dihydro-1H-inden-1-yl]-2,2-dimethylpropanamide (110. mg, 0.377 mmol, prepared in Step B), (6S)-3-iodo-5,7-dihydrospiro[cyclopenta[b]pyridine-6,3′-pyrrolo[2,3-b]pyridin]-2′(1′H)-one (137 mg, 0.377 mmol, Intermediate 7) and N,N-dicyclohexylmethylamine (81.0 mg, 0.415 mmol) in DMF (3.77 mL) was added bis-(tri-1-butylphosphine) palladium(0) (57.8 mg, 0.113 mmol). This solution was once again degassed, before being sealed and heated in a microwave at 120° C. for 20 minutes. The reaction mixture was then diluted with DCM and washed twice with half-saturated brine. The organics were dried over sodium sulfate, filtered, and concentrated in vacuo to provide a residue. The residue was then applied to a silica gel column for purification, eluting with a gradient of 1-7% MeOH in DCM to provide the title compound. MS: m/z=527 (M+1).

1. customThis solution was once again degassed
2. custombefore being sealed
3. additionThe reaction mixture was then diluted with DCM
4. washwashed twice with half-saturated brine
5. dry with materialThe organics were dried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customto provide a residue
9. customThe residue was then applied to a silica gel column for purification
10. washeluting with a gradient of 1-7% MeOH in DCM