HRID733147

反应详情

EQUATION

反应方程式

HRID 733147 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3-chloro-4-fluorophenylhydrazine (2 g, 12.4 mmol) and ethyl-2,4-dioxovalerate (2.36 g, 14.9 mmol) in ethanol (40 ml) was refluxed for 16 hours, then cooled to room temperature and partitioned between EtOAc and water. The organic layer was washed with saturated bicarbonate, brine solution, dried over sodium sulfate, filtered, concentrated and purified by silica-gel column chromatography using 4% EtOAc in heaxanes to give the product (2.45 g, 71%) as a solid.

WORKUP

后处理

  1. custompartitioned between EtOAc and water
  2. washThe organic layer was washed with saturated bicarbonate, brine solution
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. custompurified by silica-gel column chromatography