Dimethylformamide → Ethyl 3-(chlorocarbonyl)-5-nitrobenzoate

HRID 1422407노트

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HRID 1422407 반응식
[CH2:1]([O:3][C:4](=[O:17])[C:5]1[CH:13]=[C:12]([N+:14]([O-:16])=[O:15])[CH:11]=[C:7]([C:8](O)=[O:9])[CH:6]=1)[CH3:2].C(Cl)(=O)C([Cl:21])=O.CN(C=O)C>C(Cl)Cl>[CH2:1]([O:3][C:4](=[O:17])[C:5]1[CH:13]=[C:12]([N+:14]([O-:16])=[O:15])[CH:11]=[C:7]([C:8]([Cl:21])=[O:9])[CH:6]=1)[CH3:2]

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 65578Oxalyl chlorideHCID 898721,3-Benzenedicarboxylic acid, 5-nitro-, 1-ethyl ester

생성물 1

HCID 3023043Ethyl 3-(chlorocarbonyl)-5-nitrobenzoate

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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).

후처리

  1. concentrationconcentrated in vacuum
  2. customThe residue was triturated with toluene
  3. concentrationagain concentrated in vacuum

출처 및 근거

ORD 기록
ord-00384f123a3c4034ad603224e8256ae0
출처 데이터셋
uspto-grants-2015_01
특허 번호
USRE045323E1

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