HRID357551

反应详情

EQUATION

反应方程式

HRID 357551 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

11.9 g of the 4-(2-hydroxyethoxy)-2-hydroxymethyl-3-methylpyridine prepared above was dissolved in 200 ml of dichloromethane to obtain a solution. 24 ml of thionyl chloride was dropwise added to this solution at 0° C. The obtained mixture was stirred at a room temperature for 2 hours and distilled under a reduced pressure to remove the dichloromethane and excess thionyl chloride. A saturated aqueous solution of sodium hydrogencarbonate was added to the residue to obtain a mixture. This mixture was extracted with chloroform. The extract was dried over magnesium sulfate and filtered. The filtrate was concentrated to obtain 10.9 g of 2-chloromethyl-4-(2-hydroxyethoxy)-3-methylpyridine.

WORKUP

后处理

  1. customto obtain a solution
  2. distillationdistilled under a reduced pressure
  3. customto remove the dichloromethane and excess thionyl chloride
  4. additionA saturated aqueous solution of sodium hydrogencarbonate was added to the residue
  5. customto obtain a mixture
  6. extractionThis mixture was extracted with chloroform
  7. dry with materialThe extract was dried over magnesium sulfate
  8. filtrationfiltered
  9. concentrationThe filtrate was concentrated