HRID13742

反应详情

EQUATION

反应方程式

HRID 13742 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Into a two-liter four-necked flask provided with a stirrer, a thermometer, dropping device, a hydrochloric-acid-recovering device and a condenser, 213.4 g (1.1 moles) of dibutylphosphite, 5.6 g (0.06 moles) of triethylamine and 1.05 g (0.011 moles) of magnesium chloride were fed. While stirring the resulting mixed solution at 25° C., 120.0 g (1.2 moles) of methyl isobutyl ketone (MIBK) was added thereto in 1 hour. The resulting mixed solution was further stirred for 1 hour at the same temperature (25° C.) to complete the reaction. Thereafter, the mixed solution was washed to remove the low-boiling point portions, as in (synthesis of raw material 2) of Example 1, and thus, the triethylamine and the magnesium chloride was removed from the mixed solution, to obtain 298.8 g of dibutyl(1-hydroxy-1,3-dimethylbutyl)phosphonate (raw material 3).

WORKUP

后处理

  1. customInto a two-liter four-necked flask provided with a stirrer
  2. additionmixed solution at 25° C.
  3. additionThe resulting mixed solution
  4. stirringwas further stirred for 1 hour at the same temperature (25° C.)
  5. customthe reaction
  6. washThereafter, the mixed solution was washed
  7. customto remove the low-boiling point portions
  8. customas in (synthesis of raw material 2) of Example 1
  9. customthus, the triethylamine and the magnesium chloride was removed from the mixed solution