HRID1023450
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
- 85 °C
PROCEDURE
实验过程
Potassium carbonate (93.2 mg, 0.674 mmol) is added to a solution of the crude 1-benzoyl-3-{4-[2-(2-methoxy-phenyl)-ethyl]-pyridin-2-yl}-urea (211 mg) in absolute ethanol (3 mL), and the mixture is heated at 85° C. After 2 hours, the mixture is cooled to room temperature, neutralized with 1 M aqueous HCl to pH 7-8, and stirred over night. The mixture is filtered, and the solids are washed with EtOH (2×0.5 mL) and air dried. The solids are partitioned between ethyl acetate (10 mL) and saturated aqueous NaHCO3 (3 mL). The organic layer is dried over MgSO4, filtered and concentrated to give the titled product.
WORKUP
后处理
- temperaturethe mixture is cooled to room temperature
- filtrationThe mixture is filtered
- washthe solids are washed with EtOH (2×0.5 mL) and air
- customdried
- customThe solids are partitioned between ethyl acetate (10 mL) and saturated aqueous NaHCO3 (3 mL)
- dry with materialThe organic layer is dried over MgSO4
- filtrationfiltered
- concentrationconcentrated