HRID1067597

反应详情

EQUATION

反应方程式

HRID 1067597 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.07 g of ethyl 2-(6-chloroimidazo[1,2-b]pyridazin-2-yl)-2-methylpropionate was suspended in 60 ml of ethyl acetate; 2.13 g of N-chlorosuccinimide was added, followed by thermal refluxing for 4 hours. After cooling, water was added, followed by extraction with ethyl acetate; the extract was washed with saturated saline and dried with magnesium sulfate. The dry product was concentrated under reduced pressure; the residue was subjected to silica gel column chromatography and eluted with hexane:ethyl acetate (5:1). The desired fraction was collected and concentrated under reduced pressure to yield 4.48 g of the title compound.

WORKUP

后处理

  1. customrefluxing for 4 hours
  2. temperatureAfter cooling
  3. extractionfollowed by extraction with ethyl acetate
  4. washthe extract was washed with saturated saline
  5. dry with materialdried with magnesium sulfate
  6. concentrationThe dry product was concentrated under reduced pressure
  7. washeluted with hexane:ethyl acetate (5:1)
  8. customThe desired fraction was collected
  9. concentrationconcentrated under reduced pressure