HRID2050585

反应详情

EQUATION

反应方程式

HRID 2050585 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 (E)-3-[4,5-bis(4-fluorophenyl)-2-(1-methylethyl)-1H-imidazol-1-yl]-2-propenal (430 mg) in dry THF (7 ml) at 0° under nitrogen, allylmagnesium chloride (2M in THF, 0.86 ml) was added. The mixture was stirred for 2.5 h at 0° and then quenched with saturated aqueous ammonium chloride. Extraction with ether (4×) gave, after drying and rotary-evaporation, the crude product (466 mg). FCC eluting with 20% then 30% System A afforded the title product (331.9 mg) as a white solid. Rf 0.41 (System A 1:1); νmax (CHBr3) 3587 cm-1 (OH).

WORKUP

后处理

  1. customquenched with saturated aqueous ammonium chloride
  2. extractionExtraction with ether (4×)
  3. customgave
  4. customafter drying
  5. customrotary-evaporation
  6. washFCC eluting with 20%