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