HRID465441

反应详情

EQUATION

反应方程式

HRID 465441 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-hydroxyphenylpropan-2-one, ethylene ketal (4.7 g), potassium carbonate (3.5 g) and chloroacetonitrile (1.83 g) in acetone, was heated under reflux for 5 h, cooled, filtered, and treated with 2N hydrochloric acid (1 ml). The solution was allowed to stand at room temperature for 4 h, the solvent was evaporated in vacuo and the residue partitioned between ethylacetate and water. The organic layer was dried, (magnesium sulphate), filtered and evaporated. The residue was purified by column chromatography on silica using chloroform as eluent to give 4-acetonylphenoxyacetonitrile, (3.0 g)

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 5 h
  3. temperaturecooled
  4. filtrationfiltered
  5. additiontreated with 2N hydrochloric acid (1 ml)
  6. customthe solvent was evaporated in vacuo
  7. customthe residue partitioned between ethylacetate and water
  8. dry with materialThe organic layer was dried, (magnesium sulphate),
  9. filtrationfiltered
  10. customevaporated
  11. customThe residue was purified by column chromatography on silica