HRID33577

反应详情

EQUATION

反应方程式

HRID 33577 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To an ice/salt cooled solution of 1-fluoronaphthalene (5.1 g) in anhydrous dichloromethane (20 ml) was added aluminium chloride (5.6 g). After 5 minutes, a solution of isovaleryl chloride (4.2 g) in anhydrous dichloromethane (5 ml) was added dropwise over 20 minutes. The mixture was allowed to warm to room temperature overnight, then added cautiously to a vigorously stirred mixture of ice water and dichloromethane. The organic layer was separated, clarified with methanol, washed with brine, dried with sodium sulphate, filtered and evaporated in vacuo. The title compound (7 g) was obtained following silica gel column chromatography of the residue in 20-40% dichloromethane in petroleum ether.

WORKUP

后处理

  1. customThe organic layer was separated
  2. washwashed with brine
  3. dry with materialdried with sodium sulphate
  4. filtrationfiltered
  5. customevaporated in vacuo