HRID223661

反应详情

EQUATION

反应方程式

HRID 223661 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

327 mg. of 2-[(2,6-dichlorophenyl)imino]-1-hydroxyimidazolidine hydrobromide are dissolved in 5 ml. of absolute dimethylformamide, and 90 mg. of sodium hydride are added at 5°. The solution is stirred at room temperature until it becomes clear and is cooled again down to 5° and 1.2 ml. of a 1.0 molar methyl iodide solution in dimethylformamide are added. After 30 minutes, the reaction product is poured onto water and the aqueous phase is extracted twice with ether. The organic extracts are dried and evaporated in vacuo. The residue is dissolved in 1 ml. of acetonitrile, and hydrogen chloride in dioxane is added. The 2-[(2,6-dichlorophenyl)imino]-1-methoxyimidazolidine hydrochloride which has precipitated melts at 228°.

WORKUP

后处理

  1. temperatureis cooled again down to 5° and 1.2 ml
  2. additionthe reaction product is poured onto water
  3. extractionthe aqueous phase is extracted twice with ether
  4. customThe organic extracts are dried
  5. customevaporated in vacuo
  6. dissolutionThe residue is dissolved in 1 ml
  7. additionof acetonitrile, and hydrogen chloride in dioxane is added
  8. customThe 2-[(2,6-dichlorophenyl)imino]-1-methoxyimidazolidine hydrochloride which has precipitated melts at 228°