HRID414477

反应详情

EQUATION

反应方程式

HRID 414477 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

N-[2-(9-anthryloxy)ethyl]phthalimide (6.5 g) was refluxed for 3 hours in ethanol containing 85% hydrazine hydrate (3.0 ml). The solution was cooled and diluted with ethyl acetate. The resultant solution was washed with dilute aqueous potassium hydroxide, dried and evaporated. The crude product was chromatographed on 300 g silica gel, eluting with a solution of methylene chloride:methanol:ammonium hydroxide, 95:4:1, yielding 1-(9-anthryloxy)-2-aminoethane, which was converted to the maleate, mp 190°-195° C., according to the method of Example 3.

WORKUP

后处理

  1. temperatureThe solution was cooled
  2. washThe resultant solution was washed with dilute aqueous potassium hydroxide
  3. customdried
  4. customevaporated
  5. customThe crude product was chromatographed on 300 g silica gel
  6. washeluting with a solution of methylene chloride