HRID1656646

反应详情

EQUATION

反应方程式

HRID 1656646 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-amino-7-hydroxytetralin (1.9 g) and 1-(2-chlorophenoxy)-2,3-epoxypropane (2.15 g) in absolute ethanol (60 ml) is refluxed for 5 hours and then ethanol is evaporated off under reduced pressure. The thus obtained residue is chromatographed on a silica gel column eluting first with ethyl acetate up to the complete elution of the first spot and then with a mixture ethyl acetate/methanol 9/1 v/v. The obtained fractions are pooled and concentrated to dryness. The residue is dissolved in isopropanol (20 ml) and the obtained solution is acidified by the addition of HC1/isopropanol. The precipitate is recovered by filtration yielding 2.25 g of N-(7-hydroxy-1,2,3,4-tetrahydronaphth-2-yl)-2-hydroxy-3-(2-chlorophenoxy)propanamine hydrochloride; m.p. 201°-203° C.

WORKUP

后处理

  1. temperatureis refluxed for 5 hours
  2. customethanol is evaporated off under reduced pressure
  3. customThe thus obtained residue is chromatographed on a silica gel column
  4. washeluting first with ethyl acetate up to the complete elution of the first spot
  5. concentrationconcentrated to dryness
  6. dissolutionThe residue is dissolved in isopropanol (20 ml)
  7. additionthe obtained solution is acidified by the addition of HC1/isopropanol
  8. filtrationThe precipitate is recovered by filtration