HRID2075647

反应详情

EQUATION

反应方程式

HRID 2075647 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To an ice-cooled solution of Compound 44 (2.81 g, 3.44 mmol) in THF (30 ml), a solution of 1M tetrabutylammonium fluoride in THF (4 ml) was added. After completion of the addition, the ice bath was removed, and this was followed by stirring at room temperature for 1 hour. This was poured over water to stop the reaction, after which extraction from ethyl acetate was conducted. The organic phases were combined and washed with saturated brine, thereafter dried with anhydrous sodium sulfate. Filtration and concentration under reduced pressure were conducted, after which the residue obtained was purified by silica gel column chromatography (Yamazen YFLC Gel, eluent (n-hexane:ethyl acetate 1:1-1:2-1:3)) to yield Compound 45 (light-yellow oil 1.95 g, 96%).

WORKUP

后处理

  1. additionAfter completion of the addition
  2. customthe ice bath was removed
  3. additionThis was poured over water
  4. customthe reaction
  5. extractionafter which extraction from ethyl acetate
  6. washwashed with saturated brine
  7. dry with materialdried with anhydrous sodium sulfate
  8. filtrationFiltration and concentration under reduced pressure
  9. customafter which the residue obtained
  10. customwas purified by silica gel column chromatography (Yamazen YFLC Gel, eluent (n-hexane:ethyl acetate 1:1-1:2-1:3))