HRID220350

反应详情

EQUATION

反应方程式

HRID 220350 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-(3-Benzoylthioureido)-N,N-dicyclopropyl-6-ethyl-1-methyl-1,6-dihydroimidazo[4,5-d]pyrrolo[2,3-b]pyridine-7-carboxamide (example 2A, 306 mg, 0.61 mmol) and 1N NaOH (10 ml, 10.00 mmol) in 10 ml EtOH were heated at 60° C. for 1 h. The reaction was cooled to room temperature and concentrated. The remaining aqueous solution was extracted (3×) with ethyl acetate. The organic phase was dried over Na2SO4, filtered, and concentrated. Purification by silica gel chromatography (dichloromethane/methanol 0-4%) gave N,N-dicyclopropyl-6-ethyl-1-methyl-4-thioureido-1,6-dihydroimidazo[4,5-d]pyrrolo[2,3-b]pyridine-7-carboxamide as a yellow solid (199 mg, 82% yield).

WORKUP

后处理

  1. concentrationconcentrated
  2. extractionThe remaining aqueous solution was extracted (3×) with ethyl acetate
  3. dry with materialThe organic phase was dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customPurification by silica gel chromatography (dichloromethane/methanol 0-4%)