HRID80598

反应详情

EQUATION

反应方程式

HRID 80598 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To ethyl 2-(bromomethyl)acrylate (104.4 g) in an acetonitrile (900 ml) solution, di-tert-butyl imino dicarboxylate (122.4 g) and potassium carbonate was added, and the mixture was stirred at room temperature for 2 days. The reaction solution was concentrated in vacuo. To the residue, ethyl acetate (1.4 liter) and water (700 ml) were added, and the layers were separated. The organic layer was washed with water (350 ml), dried over sodium sulfate, then concentrated to obtain ethyl 2-{[di(tert-butoxycarbonyl)amino]methyl}acrylate (compound S62a) as a crude product (182.7 g).

WORKUP

后处理

  1. concentrationThe reaction solution was concentrated in vacuo
  2. additionTo the residue, ethyl acetate (1.4 liter) and water (700 ml) were added
  3. customthe layers were separated
  4. washThe organic layer was washed with water (350 ml)
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated