HRID434548

反应详情

EQUATION

反应方程式

HRID 434548 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 2.00 g (13.4 mmoles) of D-penicillamine and 1.73 g (13.4 mmoles) of N,N-dimethylacetoacetamide in 15 ml of dry benzene, and 0.6 g of anhydrous magnesium sulfate was refluxed for 3.5 hours under a stream of argon. The reaction mixture became clear and then the solvent was distilled off. The resulting residue was dissolved in hot methyl alcohol. Insolubles were removed by filtration and the solvent was again distilled off. The residue was crystallized from chloroform and further recrystallized from ethyl alcohol-ether to give 2.3 g of 4-carboxy-2,5,5-trimethylthiazolidine-2-N,N-dimethylacetamide as colorless prisms.

WORKUP

后处理

  1. temperaturewas refluxed for 3.5 hours under a stream of argon
  2. distillationthe solvent was distilled off
  3. dissolutionThe resulting residue was dissolved in hot methyl alcohol
  4. customInsolubles were removed by filtration
  5. distillationthe solvent was again distilled off
  6. customThe residue was crystallized from chloroform
  7. customfurther recrystallized from ethyl alcohol-ether