HRID229030

反应详情

EQUATION

反应方程式

HRID 229030 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-(3-Formyl-pyridin-2-yl)-2,2-dimethyl-propionamide (9.68 g) was dissolved in 3 N hydrochloric acid (140 ml), and the solution was stirred under reflux overnight. The reaction solution was cooled to room temperature, was then washed with diethyl ether, and was neutralized with potassium carbonate powder. Diethyl ether was added thereto, and the mixture was extracted. The diethyl ether layer was dried over potassium carbonate, and the solvent was removed by distillation under the reduced pressure. The residue was purified by column chromatography using acetone-chloroform to give 2-amino-pyridine-3-carbaldehyde (5.03 g, yield 88%).

WORKUP

后处理

  1. temperatureunder reflux overnight
  2. washwas then washed with diethyl ether
  3. additionDiethyl ether was added
  4. extractionthe mixture was extracted
  5. dry with materialThe diethyl ether layer was dried over potassium carbonate
  6. customthe solvent was removed by distillation under the reduced pressure
  7. customThe residue was purified by column chromatography