HRID1532795

反应详情

EQUATION

反应方程式

HRID 1532795 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

A 1 l autoclave reactor was filled with 120 g of 2-(2′,4′-dinitrophenoxy)ethanol, 3 g of a 1% platinum/carbon catalyst which included 50% water, and 400 ml of isopropanol. At a hydrogen pressure of 1 MPa and a temperature of 100° C., hydrogenation was carried out for 10 h. The system was then cooled to 20° C., and the reaction mixture was added dropwise under a nitrogen atmosphere through a filter into an initial charge of 240 g of 37% strength hydrochloric acid which had been previously flushed repeatedly with nitrogen. The resulting suspension was heated at reflux temperature for about 30 min and then cooled to 10° C. The product obtained after filtration was washed once with isopropanol to give 113.1 g of 2-(2′,4′-diamino-phenoxy)ethanol (89.1% yield) in 98% purity. Measuring the degrees of transmission of a 0.1% strength solution of the product in water in accordance with DIN 55945 gave, as results, Tx=99.4, Ty=98.9 and Tz=98.2.

WORKUP

后处理

  1. additionthe reaction mixture was added dropwise under a nitrogen atmosphere through
  2. filtrationa filter into
  3. additionan initial charge of 240 g of 37% strength hydrochloric acid which
  4. customhad been previously flushed repeatedly with nitrogen
  5. temperatureThe resulting suspension was heated
  6. temperatureat reflux temperature for about 30 min
  7. temperaturecooled to 10° C
  8. customThe product obtained
  9. filtrationafter filtration
  10. washwas washed once with isopropanol