HRID1704633

反应详情

EQUATION

反应方程式

HRID 1704633 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

850 g (3 moles) 2-(2-thienyl)-ethyl paratoluene sulfonate and 850 g (6 moles) ortho-chlorobenzylamine are dissolved in 5.2 liters acetonitrile and the mixture is refluxed during 6.5 hours. After filtration, 630 g ortho-chlorobenzylamine paratoluene sulfonate are removed by filtration. The filtrate is concentrated and the residue is taken up into diisopropyl ether and 500 ml 2N sodium hydroxide. The organic phase is separated and is made acidic with 3N hydrochloric acid. The resulting hydrochloride precipitates out; it is collected by filtration, suction filtered and washed with acetone, to give 684 g (Yield: 78%) N-(2-chloro-benzyl)-2-(2-thienyl)-ethylamine hydrochloride.

WORKUP

后处理

  1. temperaturethe mixture is refluxed during 6.5 hours
  2. filtrationAfter filtration, 630 g ortho-chlorobenzylamine paratoluene sulfonate
  3. customare removed by filtration
  4. concentrationThe filtrate is concentrated
  5. customThe organic phase is separated
  6. customThe resulting hydrochloride precipitates out
  7. filtrationit is collected by filtration, suction
  8. filtrationfiltered
  9. washwashed with acetone