反应 #1509589

ord-00384f123a3c4034ad603224e8256ae0

反应方程式

CCOC(=O)c1cc(C(=O)O)cc([N+](=O)[O-])c1
5-nitroisophtalic acid monoethyl ester
O=C(Cl)C(=O)Cl
oxalyl chloride
CN(C)C=O
DMF
CCOC(=O)c1cc(C(=O)Cl)cc([N+](=O)[O-])c1
title compound
CCOC(=O)c1cc(C(=O)Cl)cc([N+](=O)[O-])c1
3-Chlorocarbonyl-5-nitro-benzoic acid ethyl ester

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    浓缩concentrated in vacuum
  2. 2
    其他The residue was triturated with toluene
  3. 3
    浓缩again concentrated in vacuum

实验过程

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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: USRE045323E1uspto-grants-2015_01