HRID398358

反应详情

EQUATION

反应方程式

HRID 398358 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of pyridine (3.52 mL, 43.6 mmol) in CH2Cl2 (10 mL) was added dry chromium trioxide (2.18 g, 21.80 mmol) at 0° C. The reaction mixture was warmed to room temperature and stirred for 30 min. 4-fluoro-3-(1-hydroxyethyl)benzonitrile (600 mg, 3.63 mmol) dissolved in CH2Cl2 (10 mL) was added via canula. The reaction mixture was stirred for 10 min. and was diluted with ether and celite and stirred for an additional 20 min. The reaction mixture was filtered through a pad of celite and washed with ethyl acetate. The organic was washed then with 5% HCl and sat'd NaHCO3, brine, dried over MgSO4, and concentrated in vacuo to provide product:

WORKUP

后处理

  1. additionwas added via canula
  2. stirringThe reaction mixture was stirred for 10 min.
  3. stirringstirred for an additional 20 min
  4. filtrationThe reaction mixture was filtered through a pad of celite
  5. washwashed with ethyl acetate
  6. washThe organic was washed
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated in vacuo
  9. customto provide product