HRID26170

反应详情

EQUATION

反应方程式

HRID 26170 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
220 °C

PROCEDURE

实验过程

Into a 50 ml 3-neck round bottom flask fitted with a condenser, thermometer, and magnetic stirrer were placed 11.4 g (0.04 mole) stearic acid, 8.0 g (0.06 mole) N-chlorosuccinimide, 0.1 ml (0.0015 mole) chlorosulfonic acid, and 0.04 g (0.0002 mole) TCNQ. The flask was placed in a heating bath set at 150° C. The mixture was stirred during heating, and a homogeneous liquid phase was formed. The solution temperature continued to rise above that of the heating bath, and a sudden exothermic reaction occurred in which the reaction temperature increased to ca. 220° C. The reaction mixture was cooled and dissolved in chloroform, and the resulting solution was washed thoroughly with dilute aqueous sodium chloride solution. After drying and removal of the chloroform, the residue was recrystallized from acetonitrile to afford 8.9 g (70%) of 2-chlorostearic acid which was equivalent in purity to the product of Example I.

WORKUP

后处理

  1. customInto a 50 ml 3-neck round bottom flask fitted with a condenser
  2. customthermometer, and magnetic stirrer were placed
  3. customThe flask was placed in a heating bath
  4. customset at 150° C
  5. temperatureduring heating
  6. customa homogeneous liquid phase was formed
  7. customa sudden exothermic reaction
  8. temperatureThe reaction mixture was cooled
  9. washthe resulting solution was washed thoroughly with dilute aqueous sodium chloride solution
  10. customAfter drying
  11. customremoval of the chloroform
  12. customthe residue was recrystallized from acetonitrile