HRID48974

反应详情

EQUATION

反应方程式

HRID 48974 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of 2-(4-fluoro-5-nitrobenzoyl)-3-methylpyridine (7.13 g, 0.0258 mol) and glacial acetic acid at 70-80° C. is added iron powder (7.76 g, 0.130 mol) in three portions. The resultant mixture is stirred overnight at 70-80° C., cooled to room temperature and extracted three times with ethyl acetate. The combined organic layers are filtered through Celite, dried over anhydrous magnesium sulfate and concentrated in vacuo to afford the title compound as a tan solid (4.36 g, 69.8%) which is identified by NMR spectral analysis.

WORKUP

后处理

  1. extractionextracted three times with ethyl acetate
  2. filtrationThe combined organic layers are filtered through Celite
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated in vacuo