HRID2203345

反应详情

EQUATION

反应方程式

HRID 2203345 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of pyridazine (3.63 mL, 49.9 mmol) in DCM (60 mL) was added trimethylsilyl cyanide (11.99 mL, 90 mmol) and aluminum chloride (20 mg, 0.150 mmol). After stirring the reaction mixture at room temperature for 10 minutes, a solution of para-toluene sulfonyl chloride (16.38 mL, 86 mmol) in DCM (100 mL) was added dropwise via an addition funnel over 30 minutes. The resulting light orange solution was left stirring at room temperature overnight. The reaction mixture was concentrated to give a light brown solid. To this material was added EtOH (100 mL). A white precipitate formed which was filtered through a sintered funnel. The precipitate was washed with ethanol and collected. m/z=262 (M+H).

WORKUP

后处理

  1. waitThe resulting light orange solution was left
  2. stirringstirring at room temperature overnight
  3. concentrationThe reaction mixture was concentrated
  4. customto give a light brown solid
  5. customA white precipitate formed which
  6. filtrationwas filtered through a sintered funnel
  7. washThe precipitate was washed with ethanol
  8. customcollected