HRID217621

反应详情

EQUATION

反应方程式

HRID 217621 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a round bottom flask, 5-(1H-pyrrolo[2,3-b]pyridin-5-yl)-pyridine-2-carboxylic acid ethylamide (38, 71 mg, 0.27 mmol), propane-1-sulfonic acid (2,4-difluoro-3-formyl-phenyl)-amide (58, 84.2 mg, 0.32 mmol) and potassium hydroxide (44.9 mg, 0.80 mmol) were combined with 1.1 mL of methanol. The reaction was stirred for 2 hours at room temperature. The reaction solution was neutralized with 0.1 N hydrochloric acid, then extracted 3× with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate, filtered and the filtrate concentrated under vacuum. The resulting residue was purified by silica gel column chromatography to provide the desired compound (73, 55 mg). MS (ESI) [M+H+]+=530.1.

WORKUP

后处理

  1. extractionextracted 3× with ethyl acetate
  2. washThe organic layer was washed with brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationthe filtrate concentrated under vacuum
  6. customThe resulting residue was purified by silica gel column chromatography