반응 #1509589

ord-00384f123a3c4034ad603224e8256ae0

반응 방정식

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

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축concentrated in vacuum
  2. 2
    기타The residue was triturated with toluene
  3. 3
    농축again concentrated in vacuum

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: USRE045323E1uspto-grants-2015_01