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
PROCEDURE
实验过程
2-{6-[3-(2-Methoxy-phenyl)-1-(toluene-4-sulfonyl)-1H-pyrrolo[2,3-b]pyridin-5-yl]-pyrimidin-4-yl}-N,N-dimethyl-2-oxo-acetamide (100 mg, 0.179 mmole) in methanol (3.6 mL) was cooled to 0° C. in an ice bath. Potassium hydroxide (aqueous 50% w/v, 0.06 mL) was added, the solution removed from the ice bath, maintained at ambient temperature for 15 hrs, and quenched with acetic acid (0.06 mL). The resulting solution was concentrated to remove all volatile organics, dissolved in ethyl acetate (10 mL), washed with sodium bicarbonate (5 mL), then with water (5 mL), then with brine (5 mL), and dried over magnesium sulfate. The solution was filtered and concentrated to dryness to afford 2-{6-[3-(2-methoxy-phenyl)-1H-pyrrolo[2,3-b]pyridin-5-yl]-pyrimidin-4-yl}-N,N-dimethyl-2-oxo-acetamide (63 mg, 72%) as a yellow solid which was used without further purification. MS: m/z 402.2 (M+H+).
WORKUP
后处理
- customthe solution removed from the ice bath
- customquenched with acetic acid (0.06 mL)
- concentrationThe resulting solution was concentrated
- customto remove all volatile organics,
- dissolutiondissolved in ethyl acetate (10 mL)
- washwashed with sodium bicarbonate (5 mL)
- dry with materialwith water (5 mL), then with brine (5 mL), and dried over magnesium sulfate
- filtrationThe solution was filtered
- concentrationconcentrated to dryness