HRID219755

反应详情

EQUATION

反应方程式

HRID 219755 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

37.2 g (94 mMol) of the product 1a and 11.1 g (94 mMol) of zinc cyanide in 300 ml of DMF were heated to 95° C. Then 1.6 g (1.38 mMol) of tetrakis-(triphenylphosphine)palladium(0) were added in portions every 10 minutes. After 45 minutes, the reaction mixture was poured into ice-water and extracted with ethyl acetate. The organic phase was washed with saturated NaCl solution, dried and concentrated in vacuo. The residue obtained in this way crystallizes from a little ethyl acetate. 24 g of the product were obtained.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe organic phase was washed with saturated NaCl solution
  3. customdried
  4. concentrationconcentrated in vacuo
  5. customThe residue obtained in this way
  6. customcrystallizes from a little ethyl acetate