HRID2084390

反应详情

EQUATION

反应方程式

HRID 2084390 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In an argon atmosphere, 4-[4-(1H-1,2,3-triazol-1-yl)butyl]phenol (218 mg) and 65% oily sodium hydride (39 mg) were dissolved in DMF (5 ml) added thereto. With stirring under ice cooling, 4-(chloromethyl)-2-[(E)-2-(4-fluorophenyl)ethenyl]-1,3-oxazole (250 mg) was added, followed by stirring at room temperature for 3 hours. After water was added, the reaction mixture was extracted with ethyl acetate. The extract was washed with water and saturated saline and dried over sodium sulfate, after which it was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: chloroform-ethanol=24:1), after which it was recrystallized from ethyl acetate to yield the titled compound (368 mg) as colorless crystals.

WORKUP

后处理

  1. additionadded
  2. stirringby stirring at room temperature for 3 hours
  3. extractionthe reaction mixture was extracted with ethyl acetate
  4. washThe extract was washed with water and saturated saline
  5. dry with materialdried over sodium sulfate
  6. concentrationafter which it was concentrated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (eluent: chloroform-ethanol=24:1)
  8. customafter which it was recrystallized from ethyl acetate