反应详情

温度

130 °C

3-Bromo-7-(morpholine-4-carbonyl)-9H-carbazole-1-carboxamide (40 mg, 0.10 mmol, Example 144A) and dicyclohexy(2′,6′-dimethoxybiphenyl-2)phosphine (8.2 mg) were dissolved in dioxane (1.5 mL) and added into a 2-ml microwave vial containing (E)-styrylboronic acid (37 mg, 0.25 mmol), followed by addition of potassium phosphate (64 mg in 0.15 mL water) into above vials. Pd(OAc)2 (4.49 mg, 20.00 μmol) was added as solid. The vial was sealed and heated to 130° C. for 10 minutes. The crude reaction mixture was evaporated to dryness, dissolved in DMF+MeOH (1.2 mL+0.4 mL), filtered and purified by preparative HPLC. Product containing fractions were combined and evaporated to dryness to give 1.4 mg (E)-7-(morpholine-4-carbonyl)-3-styryl-9H-carbazole-1-carboxamide. HPLC retention time 4.39 min. (SUPELCO® Ascentis Express 4.5×50 mm 3 um C18, 2 ml/min, 5 to 95% B in 8 minutes, then 95% B for 1 minute. Solvent A: 5% CH3CN—95% H2O—10 mM NH4OAc; Solvent B: 95% CH3CN—5% H2O—10 mM NH4OAc). MS (ESI) m/e+=426 [M+H]+.

1. additionadded into a 2-ml microwave vial
2. customThe vial was sealed
3. customThe crude reaction mixture
4. customwas evaporated to dryness
5. dissolutiondissolved in DMF+MeOH (1.2 mL+0.4 mL)
6. filtrationfiltered
7. custompurified by preparative HPLC
8. additionProduct containing fractions
9. customevaporated to dryness