HRID1533794

反应详情

EQUATION

反应方程式

HRID 1533794 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of ethyl 3-[[1-(hydroxyimino)ethyl]amino]-pyrazole-4-carboxylate (1.50 g) and pyridine (1.12 g) in N,N-dimethylformamide (20 ml) was added dropwise p-toluenesulfonyl chloride (1.39 g) under ice bath cooling and stirred at ambient temperature for 3 hours. The reaction mixture was diluted with ethyl acetate and water. The organic layer was separated and washed with saturated sodium hydrogen carbonate aqueous solution and brine. The solution was dried over magnesium sulfate and concentrated in vacuo to give ethyl 3-[1-(p-toluenesulfonyloxyimino)ethyl]amino-1H-pyrazole-4-carboxylate (2.14 g).

WORKUP

后处理

  1. temperaturecooling
  2. customThe organic layer was separated
  3. washwashed with saturated sodium hydrogen carbonate aqueous solution and brine
  4. dry with materialThe solution was dried over magnesium sulfate
  5. concentrationconcentrated in vacuo