HRID1165282

反应详情

EQUATION

反应方程式

HRID 1165282 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2-bromo-1-[3-(methoxymethyl)-4-(phenylmethoxy)phenyl]ethanone (1.38 g), N-[6-[2-(4-methoxyphenyl)ethoxy]hexyl]benzenemethanamine (1.35 g) and DEA (1.02 g) in THF (21 ml) was allowed to stand under nitrogen for 20 h. The mixture was filtered and the filtrate evaporated in vacuo to give an oil, a solution of which in ethanol (35 ml) was hydrogenated over pre-reduced 10% PdO-C (50% aqueous, 500 mg) and 5% PtO-C (400 mg). The mixture was filtered through hyflo and evaporated in vacuo to give an oil. Purification by FCC eluting with System B (900:100:5) gave the title compound as a cream solid (0.82 g) m.p. 97.5°-98.5°.

WORKUP

后处理

  1. filtrationThe mixture was filtered
  2. customthe filtrate evaporated in vacuo
  3. customto give an oil
  4. filtrationThe mixture was filtered through hyflo
  5. customevaporated in vacuo
  6. customto give an oil
  7. customPurification by FCC
  8. washeluting with System B (900:100:5)