HRID482608

反应详情

EQUATION

反应方程式

HRID 482608 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 25 g (281 mmole) of methoxyacetonitrile in 100 ml of diethyl ether at reflux was added 250 ml (250 mmole) of 1.0M 4-chlorophenyl magnesium bromide in diethyl ether. After refluxing for 30 minutes the reaction mixture was hydrolyzed with a solution of 30 ml of concentrated sulfuric acid in 100 ml of water. The organic layer was washed with water and brine, dried over anhydrous magnesium sulfate, concentrated in vacuo, and dissolved in hexanes. The insolubles were filtered away and the resultant solution was concentrated and distilled yielding a clear liquid. bp 105°-115° C. at 1 torr. The oil solidified on standing.

WORKUP

后处理

  1. temperatureAfter refluxing for 30 minutes the reaction mixture
  2. washThe organic layer was washed with water and brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. dissolutiondissolved in hexanes
  6. filtrationThe insolubles were filtered away
  7. concentrationthe resultant solution was concentrated
  8. distillationdistilled
  9. customyielding a clear liquid