HRID414478

反应详情

EQUATION

反应方程式

HRID 414478 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-(9-Anthryloxy)ethyl chloride (5.0 g) was heated for 5 hours at 90° C. in methylene glycol (50 ml) containing dimethylamine (4.0 g) using a dry ice condenser. The solution was cooled and added to water. The resulting mixture was extracted with ethyl acetate, and the extract dried and evaporated. The crude product was chromatographed on 100 g silica gel, eluting with a solution of methylene chloride:methanol:ammonium hydroxide, 95:5:1, to yield 1-(9-anthryloxy)-2-dimethylaminoethane, which was converted to the maleate, mp 132°-134° C.

WORKUP

后处理

  1. temperatureThe solution was cooled
  2. extractionThe resulting mixture was extracted with ethyl acetate
  3. customthe extract dried
  4. customevaporated
  5. customThe crude product was chromatographed on 100 g silica gel
  6. washeluting with a solution of methylene chloride