反应详情

温度

130 °C

Benzyl 1H-imidazol-2-ylmethyl(methyl)carbamat (1.17 g, 4.76 mmol) from Part E, 1-[2-trifluoroacetamidomethyl-phenyl]-3-trifluoromethyl-6-[4-Iodo-2-fluorophenyl]-1,4,5,6-tetrahydropyrazolo-[3,4-c]-pyridin-7-one from Part D (1.63 g, 3.18 mmol), CuI (0.12 9, 20%), K2CO3 (0.66 g, 4.76 mmol), 1,10-phenanthroline (56 mg, 20%) were added together with 100 mL of DMSO. The mixture was degassed and then heated at 130° C. under N2 for 12 h. The mixture was cooled and aqueous NH4OH (200 mL of of 10% NH4OH) was added. The mixture was filtered through Celite® and washed with EtOAc. The two layers were separated and the aqueous layer was extracted with EtOAc. The combined EtOAc mixture was washed with brine, dried over MgSO4, concentrated, and chromatographed with EtOAc to give 1.34 g of the desired product (66.9%). MS (ES+): 631.3, (M+H)+.

1. customThe mixture was degassed
2. temperatureThe mixture was cooled
3. additionaqueous NH4OH (200 mL of of 10% NH4OH) was added
4. filtrationThe mixture was filtered through Celite®
5. washwashed with EtOAc
6. customThe two layers were separated
7. extractionthe aqueous layer was extracted with EtOAc
8. washThe combined EtOAc mixture was washed with brine
9. dry with materialdried over MgSO4
10. concentrationconcentrated
11. customchromatographed with EtOAc