HRID1918903

反应详情

EQUATION

反应方程式

HRID 1918903 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A Parr reactor bottle was purged with nitrogen and charged with 10% palladium on carbon (30% wet, 150 mg dry weight) and a solution of 156e (1.78 mmol) in ethanol (25 mL). The bottle was attached to a Parr hydrogenator, evacuated, charged with hydrogen gas to a pressure of 40 psi and shaken for 2 h. After this time, the hydrogen was evacuated, and the reaction mixture was filtered through a pad of Celite 521. The filter cake was washed with ethanol (2×25 mL), and the combined filtrates were concentrated to dryness under reduced pressure to afford a quantitative yield of 156f (360 mg) as yellow oil: MS (ESI+) m/z 203.1 (M+H).

WORKUP

后处理

  1. customA Parr reactor bottle was purged with nitrogen
  2. additioncharged with 10% palladium on carbon (30% wet, 150 mg dry weight)
  3. customevacuated
  4. additioncharged with hydrogen gas to a pressure of 40 psi
  5. customAfter this time, the hydrogen was evacuated
  6. filtrationthe reaction mixture was filtered through a pad of Celite 521
  7. washThe filter cake was washed with ethanol (2×25 mL)
  8. concentrationthe combined filtrates were concentrated to dryness under reduced pressure