HRID358261

反应详情

EQUATION

反应方程式

HRID 358261 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 1.59 gm of 4-(4-aminophenyl)-1-H-imidazole and 2.22 gm of triethylorthoformate was heated for 30 minutes at 100° C. in the presence of a catalytic amount of 96% H2SO4. A 33% solution of methylamine in ethanol (9.5 gm) was then added dropwise to the cooled reaction mixture. The solution was stirred at room temperature for twenty hours and then evaporated to dryness. The residue obtained was dissolved in 10% hydrochloric acid, and the acid solution was washed with ethyl acetate and then adjusted to pH 10 with 10% NaOH. The product which separated was extracted with ethyl acetate to yield, after evaporation of the solvent, 0.45 gm of the desired compound.

WORKUP

后处理

  1. customevaporated to dryness
  2. customThe residue obtained
  3. washthe acid solution was washed with ethyl acetate
  4. customThe product which separated
  5. extractionwas extracted with ethyl acetate
  6. customto yield
  7. customafter evaporation of the solvent, 0.45 gm of the desired compound