HRID584890

反应详情

EQUATION

反应方程式

HRID 584890 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

8.8 g (29 mmol) of N-(3-bromo benzyl)-N-methylbenzamide, 8.7 g (58 mmol) of 4-formylbenzene-boronic acid and 125 ml of toluene are introduced into a three-necked flask under argon. 36 ml (72 mmol) of aqueous potassium carbonate solution (2M) are added dropwise, the reaction medium is degassed with argon and 1 g of tetrakis(triphenylphosphine)palladium(0) chloride is added with heating at 90° C. for 24 hours. The reaction medium is poured into water and extracted with dichloromethane, and the organic phase is separated out after settling of the phases has taken place, dried over magnesium sulfate and evaporated. The residue obtained is purified by chromatography on a column of silica eluded with a mixture of heptane and ethyl acetate (50/50). After evaporation of the solvents, 7.2 g (75%) of the expected product are collected.

WORKUP

后处理

  1. customthe reaction medium is degassed with argon and 1 g of tetrakis(triphenylphosphine)palladium(0) chloride
  2. additionis added
  3. additionThe reaction medium is poured into water
  4. extractionextracted with dichloromethane
  5. customthe organic phase is separated out
  6. dry with materialdried over magnesium sulfate
  7. customevaporated
  8. customThe residue obtained
  9. customis purified by chromatography on a column of silica
  10. additioneluded with a mixture of heptane and ethyl acetate (50/50)
  11. customAfter evaporation of the solvents, 7.2 g (75%) of the expected product
  12. customare collected