HRID14327

反应详情

EQUATION

反应方程式

HRID 14327 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

[2-(3-Benzyloxy-5-fluoro-phenyl)-1-oxiranyl-ethyl]-carbamic acid tert-butyl ester (3.33 g, 8.59 mmol) and m-ethyl benzylamine (2.32 g, 17.19 mmol) were dissolved in isopropyl alcohol (80 ml) and brought to reflux for 2 h. Reaction mixture was then concentrated in vacuo to remove isopropyl alcohol. Dissolved yellow liquid in ethyl acetate (30 ml), then washed with 1N HCl (3×100 ml). Aqueous layers were combined then extracted with ethyl acetate (2×100 ml). Organic layers were washed with 10% sodium bicarbonate (aq., 3×100 ml), followed by a brine wash. Organic layer was dried over sodium sulfate, filtered, then concentrated in vacuo, yielding the product (4.31 g). (ES+: 523.9)

WORKUP

后处理

  1. temperatureto reflux for 2 h
  2. customReaction mixture
  3. concentrationwas then concentrated in vacuo
  4. customto remove isopropyl alcohol
  5. dissolutionDissolved yellow liquid in ethyl acetate (30 ml)
  6. washwashed with 1N HCl (3×100 ml)
  7. extractionAqueous layers were combined then extracted with ethyl acetate (2×100 ml)
  8. washOrganic layers were washed with 10% sodium bicarbonate (aq., 3×100 ml)
  9. washwash
  10. dry with materialOrganic layer was dried over sodium sulfate
  11. filtrationfiltered
  12. concentrationconcentrated in vacuo