HRID1742062

反应详情

EQUATION

反应方程式

HRID 1742062 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.85 g (0.05 mol) of 3(5)-amino-5(3)-methyl-pyrazole in 50 ml of absolute dioxan are treated with 8.3 ml (0,06 mol) of triethylamine and then, under stirring at room temperature, are treated dropwise with a solution of 10 g (0.05 mol) of 3-nitro-benzohydroximoyl chloride in 50 ml of absolute dioxan. Stirring is continued for 3 hours and then the mixture is evaporated to dryness. The residue is treated with water and ethyl acetate. The organic phase is dried over magnesium sulphate, evaporated under vacuum and the residue obtained in this way is recrystallised from dioxan. 9.8 g (48%) of 5-amino-1-(3-nitro-benzohydroximoyl)-3-methyl-pyrazole with a m. pt. of 224° to 226° C. are obtained.

WORKUP

后处理

  1. stirringStirring
  2. customthe mixture is evaporated to dryness
  3. additionThe residue is treated with water and ethyl acetate
  4. dry with materialThe organic phase is dried over magnesium sulphate
  5. customevaporated under vacuum
  6. customthe residue obtained in this way
  7. customis recrystallised from dioxan