HRID1042609

反应详情

EQUATION

反应方程式

HRID 1042609 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

357.70 g (1.686 Mol) of 3,5-dinitrobenzoic acid are suspended in 750 ml of 1-methyl-2-pyrrolidone. The suspension is stirred up to 50° C. 386.36 g (4.599 Mol) of sodium hydrogen carbonate are added and the mixture was heated up to 90° C. 22.50 g (0.150 Mol) of sodium iodide and 204.0 ml (1.533 Mol) of 6-chlorohexanol are added to the reaction mixture which is heated to 100° C. for 1 h. After 1 h of reaction, the reaction is complete and the orange suspension is thrown on 2 l of ice and 1 l of water. The product is filtrated, washed water and dried at 50° C. under vacuum for 24 h to give 425.0 g (91%) of 6-hydroxyhexyl 3,5-dinitrobenzoate as a rose powder.

WORKUP

后处理

  1. temperaturethe mixture was heated up to 90° C
  2. temperatureis heated to 100° C. for 1 h
  3. customAfter 1 h of reaction
  4. filtrationThe product is filtrated
  5. washwashed water
  6. customdried at 50° C. under vacuum for 24 h