HRID249817

反应详情

EQUATION

反应方程式

HRID 249817 的结构方程式

PROCEDURE

实验过程

Into a round bottom flask was added 5-chloro-1-pyrrolo[2,3-b]pyridine (6, 0.524 g, 3.43 mmol, prepared as described in Example 5) in methanol (5.00 mL, 0.123 mol). Potassium hydroxide (0.800 g, 14.2 mmol) and (2,4-difluoro-3-formyl-phenyl)-carbamic acid benzyl ester (53, 1.02 g, 3.5 mmol) were added and the reaction mixture was stirred overnight. The reaction mixture was poured into 1N HCl and extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate, concentrated and crystallized from ethyl acetate to give compound 54 (710 mg, 46%). MS (ESI)[M+H+]+=444.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with brine
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated
  5. customcrystallized from ethyl acetate