反应详情

温度

130 °C

The 2-[3,5-bis(trifluoromethyl)phenyl]-N-(6′-chloro-4-methyl-3,4′-bipyridin-3′-yl)-N,2-dimethylpropanamide (D52, 77 mg, 0.15 mmol), (7S,9aS)-7-({[(1,1-dimethylethyl)(dimethyl)silyl]oxy}methyl)octahydropyrazino[2,1-c][1,4]oxazine (D51, 51.5 mg, 0.18 mmol), sodium t-Butoxide (18 mg, 0.19 mmol) were degassed together in dry toluene (1.5 mL) for 5 mins before adding Bis(dibenzyleneacetone) Palladium (9 mg, 0.015 mmol) and 2-Dicyclohexylphosphino-2′-(N′N′-dimethylamino)biphenyl (15 mg, 0.038 mmol) and heating under microwave conditions at 130° C. for 30 mins. Diluted with EtOAC, washed with sat. NaHCO3×1, brine ×1, dried (MgSO4). Filtered. Solvent evaporated. Residue purified eluting with Pent to EtOAc. No Fractions isolated clean. Mixed fractions combined, solvent evaporated and residue re-purified on a 2 g SCX column, washing with MeOH (2×10 mL) before eluting the compound off with NH3 in MeOH (3×10 mL). Solvent evaporated under reduced pressure to afford a gummy solid (86 mg).

1. additionDiluted with EtOAC
2. washwashed with sat. NaHCO3×1, brine ×1
3. dry with materialdried (MgSO4)
4. filtrationFiltered
5. customSolvent evaporated
6. customResidue purified
7. washeluting with Pent to EtOAc
8. customNo Fractions isolated clean
9. customsolvent evaporated
10. customresidue re-purified on a 2 g SCX column
11. washwashing with MeOH (2×10 mL)
12. washbefore eluting the compound off with NH3 in MeOH (3×10 mL)
13. customSolvent evaporated under reduced pressure