HRID2195010

反应详情

EQUATION

反应方程式

HRID 2195010 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
200 °C

PROCEDURE

实验过程

In a four-neck 1000 mL flask equipped with a stirrer, a thermometer, a gas inlet tube, and a Dean-Stark condenser with a water measuring trap were placed 166.2 g (1.0 mol) of diglycerin, 237.3 g (1.5 mol) of isononanoic acid, and 150 mL of toluene as a solvent. Then, the reaction mixture was heated to 200 degrees C. under a flow of nitrogen gas in a rate of 20 mL/min. At the temperature, the reaction took place while distilling off the produced water with the solvent azeotropically. When the distillation-off water subsided, the temperature was raised to 220 degrees C. to further continue the reaction. When the distillation-off water stopped, the reaction was terminated. It took about 6 hours from the start of the reaction to this point. Diglycerin isononanoate was obtained as a pale yellow viscous oil in an amount of 411.5 g (hydroxyl value: 132, acid value: 0.3).

WORKUP

后处理

  1. customIn a four-neck 1000 mL flask equipped with a stirrer
  2. customa thermometer, a gas inlet tube, and a Dean-Stark condenser with a water measuring trap were placed
  3. distillationwhile distilling off the produced water with the solvent azeotropically
  4. temperaturethe temperature was raised to 220 degrees C
  5. customthe reaction
  6. customthe reaction was terminated
  7. customIt took about 6 hours from the start of the reaction to this point