HRID2196358

反应详情

EQUATION

反应方程式

HRID 2196358 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5-cyano-3-methylpyridine-2-carboxylic acid (2 g, 12.4 mmol) in methanol (20 mL) was added thionyl chloride dropwise under reflux. The mixture was then heated at reflux with stirring. After 60 min, HPLC analysis revealed completion of reaction. To the reaction mixture was added toluene and the mixture was concentrated in vacuo to give the title compound as a pale yellow solid: ESIMS: 177; [(M+H)+]; 1H NMR (400 MHz, DMSO-d6): δ 8.92 (s, 1H), 8.39 (s, 1H), 3.90 (s, 3H), 2.46 (s, 3H).

WORKUP

后处理

  1. temperatureunder reflux
  2. temperatureThe mixture was then heated
  3. temperatureat reflux
  4. customcompletion of reaction
  5. concentrationthe mixture was concentrated in vacuo