HRID963495

反应详情

EQUATION

反应方程式

HRID 963495 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

To a mixture of 3-amino acrolein (4.52 g) and acetylacetone (7.64 g) was added catalytic amount of ammonium acetate. The mixture was heated for 19 hours at ca. 110° C., After cooling to room temperature, the mixture was poured into 100 ml of isopropyl ether and dried over magnesium sulfate. The resultant mixture was filtered off by suction in vacuo to remove an insoluble material and the filtrate was concentrated in vacuo. The crude compound was purified by column chromatography on silica gel with chloroform to give 3-acetyl-2-methylpyridine (3.58 g) as a yellow oil.

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. dry with materialdried over magnesium sulfate
  3. filtrationThe resultant mixture was filtered off by suction in vacuo
  4. customto remove an insoluble material
  5. concentrationthe filtrate was concentrated in vacuo
  6. customThe crude compound was purified by column chromatography on silica gel with chloroform