HRID2118544

反应详情

EQUATION

反应方程式

HRID 2118544 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

30.4 g (0.1 mole) of 2,4,6-trichlorophenoxyethyl bromide were added to a suspension of 48.5 g (0.5 mole) of O-ethylhydroxylamine hydrochloride in 250 ml of ethyldiisopropylamine, and the mixture was stirred for 4 days at 50° C. and then cooled to 15° C. and filtered under suction. The filtrate was evaporated down under reduced pressure, in the final stage at 60° C. and under 0.1 mbar, the residue was dissolved in 300 ml of ether, and the solution was gassed with hydrogen chloride at +3° C. 17 g of O-ethyl-N-(2,4,6-trichlorophenoxy)ethylhydroxylamine hydrochloride of melting point 173°-175° C. were obtained.

WORKUP

后处理

  1. temperaturecooled to 15° C.
  2. filtrationfiltered under suction
  3. customThe filtrate was evaporated down under reduced pressure
  4. dissolutionin the final stage at 60° C. and under 0.1 mbar, the residue was dissolved in 300 ml of ether
  5. customwas gassed with hydrogen chloride at +3° C