反応 #328873

反応方程式

5-nitroisophtalic acid monoethyl ester

oxalyl chloride

DMF

→

title compound

3-Chlorocarbonyl-5-nitro-benzoic acid ethyl ester

溶媒

DCM

DCM

反応条件

後処理

1. 1
   濃縮concentrated in vacuum
2. 2
   その他The residue was triturated with toluene
3. 3
   濃縮again concentrated in vacuum

実験手順

To a solution of 5-nitroisophtalic acid monoethyl ester (80 g) in DCM (700 ml) at 25° C. was added 2M oxalyl chloride solution in DCM (63 ml), and DMF (5 ml). The reaction was stirred for 2 h and then concentrated in vacuum. The residue was triturated with toluene and again concentrated in vacuum leaving the title compound (60 g). Rt=1.40 min for derivatised methylester (method D).

出典