HRID1679825

反应详情

EQUATION

反应方程式

HRID 1679825 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

199 g. (1 mole) of 6-methyl-1,2,3,4-tetrahydrocarbazol-1-one dissolved in 2000 ml. of dimethylformamide are taken initially and 5.6 g. (0.1 mole) of potassium chloride dissolved in 200 ml. of water are added. Thereafter 66.1 g.=74.2 ml. (1.5 mole) of ethyleneoxide are added at room temperature and heated up to 50° C. within 30 minutes, a maximum pressure of 0.2 to 0.5 bar being generated. Stirring is done for 20 hours at 50° C., the solvent is distilled off in a vacuum, the residue stirred with a mixture of 800 ml. water and 10 ml. of glacial acetic acid, the product which took a crystalline form is filtered with suction, washed with 500 ml. water and dried at 40° C. in vacuo.

WORKUP

后处理

  1. distillationthe solvent is distilled off in a vacuum
  2. stirringthe residue stirred with a mixture of 800 ml
  3. filtrationis filtered with suction
  4. washwashed with 500 ml
  5. dry with materialwater and dried at 40° C. in vacuo