反应详情

温度

90 °C

2-[3,5-bis(trifluoromethyl)phenyl]-N-[6-chloro-4-(5-fluoro-2-methylphenyl)-3-pyridinyl]-N,2-dimethylpropanamide (D55, 50 mg, 0.094 mmol), (7S,9aS)-7-({[(1,1-dimethylethyl)(dimethyl)silyl]oxy}methyl)octahydropyrazino[2,1-c][1,4]oxazine (D51, 34 mg, 0.116 mmol) were dissolved in toluene (1.5 mL). Bis tritertbutylphosphine palladium (12.5 mg, 0.0244 mmol), followed by hexadecyltrimethylammoium chloride (204, 25% aq sol), and finally sodium hydroxide solution (0.11 mL, 50% aq sol) were added. The mixture was degassed for 5 minutes before heating at 90° C. for 2 hours. Reaction cooled to R.T., diluted with EtOAc, washed with sat NaHCO3 solution, dried (MgSO4). Filtered. Solvent evaporated to afford a yellow sticky solid. Used crude in the next step.

1. additionwere added
2. customThe mixture was degassed for 5 minutes
3. customReaction
4. temperaturecooled to R.T.
5. washwashed
6. dry with materialdried (MgSO4)
7. filtrationFiltered
8. customSolvent evaporated
9. customto afford a yellow sticky solid