HRID2084404

反应详情

EQUATION

反应方程式

HRID 2084404 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-[4-[2-(2-hydroxyethyl)-1H-imidazol-1-yl ]butyl]phenol (260 mg) in DMF (4 ml), 60% oily sodium hydride (44 mg) was added under ice cooling. After stirring at room temperature for 30 minutes, (E)-4-chloromethyl-2-[2-(2,4-difluorophenyl) ethenyl]oxazole (281 mg) was added under ice cooling. After stirring at room temperature for 3 days, water was added under ice cooling. The precipitate was collected by filtration and washed with water. The precipitate was dissolved in a mixture of ethyl acetate-THF and dried over magnesium sulfate, after which it was concentrated under reduced pressure. The residue was recrystallized from ethyl acetate-hexane to yield the titled compound (275 mg) as pale-yellow crystals.

WORKUP

后处理

  1. stirringAfter stirring at room temperature for 3 days
  2. filtrationThe precipitate was collected by filtration
  3. washwashed with water
  4. dissolutionThe precipitate was dissolved in a mixture of ethyl acetate-THF
  5. dry with materialdried over magnesium sulfate
  6. concentrationafter which it was concentrated under reduced pressure
  7. customThe residue was recrystallized from ethyl acetate-hexane