HRID886558

反应详情

EQUATION

反应方程式

HRID 886558 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customthe solution removed from the ice bath
  2. customquenched with acetic acid (0.06 mL)
  3. concentrationThe resulting solution was concentrated
  4. customto remove all volatile organics,
  5. dissolutiondissolved in ethyl acetate (10 mL)
  6. washwashed with sodium bicarbonate (5 mL)
  7. dry with materialwith water (5 mL), then with brine (5 mL), and dried over magnesium sulfate
  8. filtrationThe solution was filtered
  9. concentrationconcentrated to dryness