HRID18845

反应详情

EQUATION

反应方程式

HRID 18845 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
42.5 °C

PROCEDURE

实验过程

100 g 4-Bromomethyl-2′-cyanobiphenyl is added to 500 ml acetonitrile followed by 69 g of anhydrous potassium carbonate, 12 g potassium iodide and 65 g L-Valine methyl ester. The reaction mixture is stirred at 40-45° C. for 3-4 hours. After completion of the reaction, the reaction mixture is filtered and acetonitrile is removed under vacuum at 45-50° C. 300 ml of water and 300 ml of o-xylene are added to the residue and the layers are separated. Solution of 50 g oxalic acid in 500 ml water is added to the organic layer and stirred for about an hour and filtered. The solid is washed and then dried under vacuum at 50-55° C. (yield: 130-135 g).

WORKUP

后处理

  1. customAfter completion of the reaction
  2. filtrationthe reaction mixture is filtered
  3. customacetonitrile is removed under vacuum at 45-50° C
  4. addition300 ml of water and 300 ml of o-xylene are added to the residue
  5. customthe layers are separated
  6. additionSolution of 50 g oxalic acid in 500 ml water is added to the organic layer
  7. stirringstirred for about an hour
  8. filtrationfiltered
  9. washThe solid is washed
  10. customdried under vacuum at 50-55° C. (yield: 130-135 g)