HRID868575

反应详情

EQUATION

反应方程式

HRID 868575 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 7.66 g of the N-benzyl-2-chloro-N-isopropylacetamide in 20 ml of dry diethyl ether was added dropwise to a suspension of 1.29 g of lithium aluminum hydride in 300 ml of dry diethyl ether with stirring under ice-cooling, and the mixture was heated under reflux for 4 hours. After the reaction mixture was cooled, and to the cooled reaction mixture was added dropwise water with stirring under ice-cooling. Insoluble materials were filtered off. The filtrate was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified with silica gel column chromatography (eluent: chloroform) to obtain 3.61 g of 2-(N-isopropylbenzylamino)ethyl chloride in an oil.

WORKUP

后处理

  1. temperaturecooling
  2. temperaturethe mixture was heated
  3. temperatureunder reflux for 4 hours
  4. temperatureAfter the reaction mixture was cooled
  5. customto the cooled reaction mixture
  6. stirringwith stirring under ice-
  7. temperaturecooling
  8. filtrationInsoluble materials were filtered off
  9. dry with materialThe filtrate was dried over anhydrous magnesium sulfate
  10. concentrationconcentrated under reduced pressure
  11. customThe residue was purified with silica gel column chromatography (eluent: chloroform)