HRID732947

反应详情

EQUATION

反应方程式

HRID 732947 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of acetonitrile (2.0 mL, 38.2 mmol) in THF (50 mL) at −78° C. was added nBuLi (1.81 M in hexane, 16 mL, 28.7 mmol). The resulting slurry was kept at −78° C. for 15 min and 2,4-dichlorobenzoyl chloride (2.0 g, 9.55 mmol) was added dropwise to the acetonitrile anion. After 40 min, the reaction was quenched by addition of saturated NH4Cl (30 mL). THF was removed under reduced pressure and the suspension was filtered. The solid was washed with H2O (100 mL) and dried to give 3-(2,4-dichlorophenyl)-3-oxopropanenitrile (2.0 g, 98%, >95% purity) as a light yellow solid.

WORKUP

后处理

  1. waitAfter 40 min
  2. customthe reaction was quenched by addition of saturated NH4Cl (30 mL)
  3. customTHF was removed under reduced pressure
  4. filtrationthe suspension was filtered
  5. washThe solid was washed with H2O (100 mL)
  6. customdried