HRID855639

反应详情

EQUATION

反应方程式

HRID 855639 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 5-Fluoro-2-nitro-benzoic acid (3 g, 16,2 mmol) in 200 mL of methylene chloride was added oxalyl chloride (2.26 g, 17.8 mmol) and a drop of DMF. After stirring for 2 h, the solution was poured into concentrated NH4OH. The partial solution was poured into water, extracted with Ethyl acetate, dried (Na2SO4) and concentrated to give 5-Fluoro-2-nitro-benzamide (2.61 g, 88% yield) used without purification. LCMS m/e 185.1(M+H) 183.2 (M−H), HPLC tr=2,9 min (100%).

WORKUP

后处理

  1. extractionextracted with Ethyl acetate
  2. dry with materialdried (Na2SO4)
  3. concentrationconcentrated