HRID580561

反应详情

EQUATION

反应方程式

HRID 580561 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of sodium hydride (2.30 g) in absolute dioxane (100 ml) was added dropwise ethyl 3-methyl-2-oxo-4-pyrrolidinecarboxylate (13.68 g) with stirring at room temperature. After stirring for 30 minutes, to a reaction mixture was added benzylbromide (16.42 g) during 20 minutes, then stirred for 2 hours and allowed to stand overnight at room temperature. The reaction mixture was poured into ice-water (100 ml) and extracted with chloroform, washed with water, dried over anhydrous sodium sulfate and concentrated. The residue was purified by vacuum distillation to give ethyl 1-benzyl-3-methyl-2-oxo-4-pyrrolidinecarboxylate (16.86 g), bp 155°-185° C./2 mmHg.

WORKUP

后处理

  1. stirringAfter stirring for 30 minutes, to a reaction mixture
  2. stirringstirred for 2 hours
  3. extractionextracted with chloroform
  4. washwashed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated
  7. distillationThe residue was purified by vacuum distillation