HRID2231270

反应详情

EQUATION

反应方程式

HRID 2231270 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

N-(n-propyl)-2,4,6-trichlorophenoxyacetamide, 44.0 gm, was added to 250 ml of toluene. 28 ml of borane methyl sulfide [BH3.(CH3)2S] (2 equivalents) was then slowly added to the system. The system was heated at approximately 60° C. for 15 hours at which time reaction completion was checked by IR spectroscopy. 200 ml of methanol was then slowly added to the system. After addition of the methanol, the system was acidified by bubbling in HCl gas. Afterwards, the system was refluxed for 1 hour. The solvent was then removed by stripping. The resulting oil was dissolved in methanol which was then stripped. The oil was next dissolved in methylene chloride. The organic solution was washed with a sodium hydroxide solution and then with water. The methylene chloride was removed by stripping to give 36.3 gm of the N-(n-propyl)ethanolamine 2,4,6-trichlorophenylether, as a yellow oil.

WORKUP

后处理

  1. customby bubbling in HCl gas
  2. temperatureAfterwards, the system was refluxed for 1 hour
  3. customThe solvent was then removed by stripping
  4. dissolutionThe resulting oil was dissolved in methanol which
  5. dissolutionThe oil was next dissolved in methylene chloride
  6. washThe organic solution was washed with a sodium hydroxide solution
  7. customThe methylene chloride was removed