HRID2197657

反应详情

EQUATION

反应方程式

HRID 2197657 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

To a mixture of potassium carbonate (19 g, 138 mmol, 5 equiv.) and methyl-4-aminobutyrate (IVc) (8.5 g, 55.3 mmol, 2 equiv.) in acetonitrile (70 ml, 14 vol.) is added methyl-(R)-2-bromobutyrate (IIf) (5 g, 27.6 mmol, 1 equiv.). The suspension is stirred at 40° C. for 19 hours. The mixture is then filtered and the cake is rinsed with 50 ml of acetonitrile. The filtrate is concentrated to dryness under reduced pressure and the residue is dissolved in isopropylactetate. The resulting organic layer is washed with 60 ml of water and is concentrated under vacuum to afford methyl-4-(1-methoxycarbonylpropylamino)butyrate (VIa) as a colourless oil (5.91 g, 27.2 mmol, 98%).

WORKUP

后处理

  1. filtrationThe mixture is then filtered
  2. washthe cake is rinsed with 50 ml of acetonitrile
  3. concentrationThe filtrate is concentrated to dryness under reduced pressure
  4. dissolutionthe residue is dissolved in isopropylactetate
  5. washThe resulting organic layer is washed with 60 ml of water
  6. concentrationis concentrated under vacuum