HRID1088720

反应详情

EQUATION

反应方程式

HRID 1088720 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-bromo-1-[4-hydroxy-3-(hydroxymethyl)phenyl]ethanone (460 mg), N-[6-[3-[3-(phenylmethoxy)-2-pyridinyl]propoxy]hexyl]benzenemethanamine (800 mg) and DEA (485 mg) in THF (15 ml) was left at room temperature overnight. Water (30 ml) and ether (30 ml) were added, the phases were separated and the organic layer was re-extracted with ether (50 ml). The combined extracts were washed with water and brine, dried and concentrated to an oil which was purified by FCC eluting with ethyl acetate/triethylamine (99:1) followed by ethyl acetate/methanol/triethylamine (90:10:1) to give the title compound as an orange oil (620 mg), t.l.c. (ethyl acetate/methanol/triethylamine 80:20:1) Rf 0.66.

WORKUP

后处理

  1. customthe phases were separated
  2. extractionthe organic layer was re-extracted with ether (50 ml)
  3. washThe combined extracts were washed with water and brine
  4. customdried
  5. concentrationconcentrated to an oil which
  6. customwas purified by FCC
  7. washeluting with ethyl acetate/triethylamine (99:1)