HRID977951

反应详情

EQUATION

反应方程式

HRID 977951 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of benzylamine (43.24 g) and methylene chloride (300 ml) is cooled with ice-water, and a solution of ethoxycarbonylacetyl chloride (29.63 g) in methylene chloride (150 ml) is added dropwise thereto. The mixture is stirred at the same temperature for 2 hours. The mixture is filtered to remove precipitates (benzylamine hydrochloride). The filtrate is washed with 2% hydrochloric acid and a saturated sodium chloride solution, dried and then evaporated to remove the solvent. The residue is recrystallized from a mixture of ether and n-hexane, whereby ethyl (N-benzylcarbamoyl)acetate (42.15 g) is obtained as colorless needles. Yield: 96.8%.

WORKUP

后处理

  1. filtrationThe mixture is filtered
  2. customto remove
  3. customprecipitates (benzylamine hydrochloride)
  4. washThe filtrate is washed with 2% hydrochloric acid
  5. dry with materiala saturated sodium chloride solution, dried
  6. customevaporated
  7. customto remove the solvent
  8. customThe residue is recrystallized from a mixture of ether and n-hexane