HRID1108776

反应详情

EQUATION

反应方程式

HRID 1108776 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl 3-(3-aminocyclohexyl)phenoxyacetate (8.47 g) was dissolved in ethanol (50 ml), and (R)-3-chlorostyrene oxide (4.72 g) was added prior to heating to reflux for 7.5 hours. After allowing the mixture to cool, the solvent was concentrated under reduced pressure to obtain an oily substance which was then separated and purified by silica gel column chromatography (n-hexane:ethyl acetate=1:5), to give 8.15 g of (1R)-1-(3-chlorophenyl)-2-[3-(3-ethoxycarbonylmethoxyphenyl) cyclohexylamino]ethanol (trans-H) (compound of Example 11) as an oily substance (61.8% yield).

WORKUP

后处理

  1. temperatureto heating
  2. temperatureto reflux for 7.5 hours
  3. temperatureto cool
  4. concentrationthe solvent was concentrated under reduced pressure
  5. customto obtain an oily substance which
  6. customwas then separated
  7. custompurified by silica gel column chromatography (n-hexane:ethyl acetate=1:5)