反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionthe reaction mixture was added dropwise under a nitrogen atmosphere through
- filtrationa filter into
- additionan initial charge of 240 g of 37% strength hydrochloric acid which
- customhad been previously flushed repeatedly with nitrogen
- temperatureThe resulting suspension was heated
- temperatureat reflux temperature for about 30 min
- temperaturecooled to 10° C
- customThe product obtained
- filtrationafter filtration
- washwas washed once with isopropanol