反应详情

温度

90 °C

2-Bromo-6-chloro-4-(trifluoromethyl)benzaldehyde (3.4 g, 11.9 mmol) (as described in Example 72, STEP C), ethyl 3-(5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)picolinamido)propanoate (5.0 g, 14.3 mmol), Pd(dppf)Cl2 (435 mg, 0.6 mmol), and 2 M K2CO3 (aq) (11.9 mL, 23.8 mmol) were dissolved in 1,4-dioxane (48 mL) and heated to 90° C. After 2 h the temperature was lowered to 80° C. After 14 h the resulting mixture was concentrated, diluted with EtOAc and 4M aqueous NaCl, and the layers were separated. The aqueous layer was extracted with EtOAc and the combined organics were dried (Na2SO4), concentrated, and purified via column chromatography to yield the title compound.

1. concentrationAfter 14 h the resulting mixture was concentrated
2. additiondiluted with EtOAc and 4M aqueous NaCl
3. customthe layers were separated
4. extractionThe aqueous layer was extracted with EtOAc
5. dry with materialthe combined organics were dried (Na2SO4)
6. concentrationconcentrated
7. custompurified via column chromatography