HRID461441

反应详情

EQUATION

反应方程式

HRID 461441 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 73 grams (0.275 mole) of 2,6-dichloro-4-(trichloromethyl)pyridine dissolved in 125 milliliters of acetone was added a solution of 108 grams (0.48 mole) of stannous chloride hydrate and 40 milliliters of concentrated hydrochloride acid in 500 milliliters of acetone. The mixture was refluxed for 2.0 hours. The solid which formed was separated by filtration and three fourths of the solvent was thereafter removed by evaporation. The remainder of the reaction mixture was diluted with water and the oil phase which formed, removed by extraction with hexane. The 2,6-dichloro-4-(dichloromethyl)pyridine product was dried and recovered from the solvent by evaporation of the solvent. The product had a boiling point of 123°- 126° C. at 1.6 millimeters of mercury.

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 2.0 hours
  2. customThe solid which formed
  3. customwas separated by filtration and three fourths of the solvent
  4. customwas thereafter removed by evaporation
  5. additionThe remainder of the reaction mixture was diluted with water
  6. customthe oil phase which formed
  7. customremoved by extraction with hexane
  8. dry with materialThe 2,6-dichloro-4-(dichloromethyl)pyridine product was dried
  9. customrecovered from the solvent by evaporation of the solvent