HRID2377198

反应详情

EQUATION

反应方程式

HRID 2377198 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

12 g (28 mmol) of methyl 4-benzyloxy-3-tert-butyl-5-iodobenzoate are dissolved with 5.8 g (42 mmol) of 4-methylbenzeneboronic acid and 12.7 g (84 mmol) of caesium fluoride in 400 mL of dioxane. The reaction medium is degassed with a flow of nitrogen for 15 minutes, and 1.7 g (1.4 mmol) of tetrakis(triphenylphosphine)palladium are then added. The reaction medium is refluxed for 4 hours and then cooled and hydrolysed. After extraction with ethyl acetate, the organic phase is filtered and concentrated. The residue is purified by chromatography (eluent: 98 heptane/2 ethyl acetate): a colorless oil is obtained (m=9 g, yield=83%).

WORKUP

后处理

  1. customThe reaction medium is degassed with a flow of nitrogen for 15 minutes
  2. temperatureThe reaction medium is refluxed for 4 hours
  3. temperaturecooled
  4. extractionAfter extraction with ethyl acetate
  5. filtrationthe organic phase is filtered
  6. concentrationconcentrated
  7. customThe residue is purified by chromatography (eluent: 98 heptane/2 ethyl acetate)
  8. customa colorless oil is obtained (m=9 g, yield=83%)