HRID20248

反应详情

EQUATION

反应方程式

HRID 20248 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

85 g of 2-chloro-3-cyanopyridine, 98.2 g potassium carbonate anhydrous powder and 600 g of dimethyl formamide were mixed to obtain a suspension. To this suspension, a solution of 79.2 g benzyl mercaptan in 250 ml dimethyl formamide was added dropwise over a period of approx. 3 hours at 80-90° C. The reaction mass was agitated for 2 hours at the same temperature. The temperature was slowly raised to 120° C. Then, the reaction mixture was reacted at 120-130° C. for about 1.5 hours. Afterwards, heating was stopped and reaction mass was allowed to attain the room temperature. Inorganic cake was separated by filtration. Dimethyl formamide was distilled under reduced pressure, and the residue left at bottom was 2-(phenyl methyl thio)-3-cyano pyridine 150 g, sufficiently pure to be used in the next step.

WORKUP

后处理

  1. customto obtain a suspension
  2. customThen, the reaction mixture was reacted at 120-130° C. for about 1.5 hours
  3. temperatureAfterwards, heating
  4. customreaction mass
  5. customthe room temperature
  6. customInorganic cake was separated by filtration
  7. distillationDimethyl formamide was distilled under reduced pressure
  8. waitthe residue left