反应详情

温度

100 °C

To a solution of 1-(5-bromo-4-methyl-pyridin-2-yl)-4-isopropyl-piperazine (0.59 g, 2 mmol) in 1,4-dioxane (12 mL) and water (3 mL) was added 3-acetylamino-phenylboronic acid (430 mg, 2.4 mmol), Pd(PPh3)4 (231 mg, 0.2 mmol) and TEA (404 mg, 4 mmol). The resulting mixture was degassed and heated at 100° C. for 4 h under a nitrogen atmosphere. The mixture was diluted with EtOAc and water. The organic layer was separated and the aqueous phase was extracted with EtOAc. The combined organic layers were washed with brine, dried (Na2SO4), concentrated and purified by chromatography on silica gel eluting with CH2Cl2/MeOH (100:1). This afforded 138 mg (15%) of the title compound.

1. customThe resulting mixture was degassed
2. additionThe mixture was diluted with EtOAc and water
3. customThe organic layer was separated
4. extractionthe aqueous phase was extracted with EtOAc
5. washThe combined organic layers were washed with brine
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated
8. custompurified by chromatography on silica gel eluting with CH2Cl2/MeOH (100:1)