反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 90 °C
PROCEDURE
实验过程
2-(2-Chloro-5-(trifluoromethyl)pyridin-4-ylamino)-6-methoxy-N-methylbenzamide (305 mg, 0.85 mmol), 1,3-dimethylpyrazol-5-amine (94 mg, 0.85 mmol), palladium(II) acetate (15.23 mg, 0.07 mmol), 9,9-dimethyl-4,5-bis(diphenylphosphino)xanthene (78 mg, 0.14 mmol) and cesium carbonate (331 mg, 1.02 mmol) were mixed together in dioxane (6 mL). The reaction mixture was degassed with argon and was stirred at 90° C. for 8 hours under argon. After cooling, the reaction mixture was filtered and washed with DCM. The filtrate was concentrated to dryness and was purified by flash chromatography on silica gel eluting with 1 to 5% MeOH in DCM. The solvent was evaporated to dryness to afford the title compound (118 mg, 32%) as a pale beige-pink solid.
WORKUP
后处理
- customThe reaction mixture was degassed with argon
- temperatureAfter cooling
- filtrationthe reaction mixture was filtered
- washwashed with DCM
- concentrationThe filtrate was concentrated to dryness
- customwas purified by flash chromatography on silica gel eluting with 1 to 5% MeOH in DCM
- customThe solvent was evaporated to dryness