HRID434548
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas refluxed for 3.5 hours under a stream of argon
- distillationthe solvent was distilled off
- dissolutionThe resulting residue was dissolved in hot methyl alcohol
- customInsolubles were removed by filtration
- distillationthe solvent was again distilled off
- customThe residue was crystallized from chloroform
- customfurther recrystallized from ethyl alcohol-ether