Oxalyl chloride → 2-Chloro-4-fluoro-5-nitrobenzoyl chloride

HRID 48959노트

반응식

HRID 48959 반응식
[Cl:1][C:2]1[CH:10]=[C:9]([F:11])[C:8]([N+:12]([O-:14])=[O:13])=[CH:7][C:3]=1[C:4](O)=[O:5].C(Cl)(=O)C([Cl:18])=O>CN(C)C=O.ClCCCl>[Cl:1][C:2]1[CH:10]=[C:9]([F:11])[C:8]([N+:12]([O-:14])=[O:13])=[CH:7][C:3]=1[C:4]([Cl:18])=[O:5]

참가 물질

5

반응물 2

HCID 65578Oxalyl chlorideHCID 72108282-Chloro-4-fluoro-5-nitrobenzoic Acid

생성물 1

HCID 151243842-Chloro-4-fluoro-5-nitrobenzoyl chloride

시약·촉매·용매 2

HCID 6228Dimethylformamide촉매HCID 111,2-Dichloroethane용매

실험 절차

A mixture of 2-chloro-4-fluoro-5-nitrobenzoic acid (50.0 g, 0.228 mol) and N,N-dimethylformamide (5 drops) in 1,2-dichloroethane is treated dropwise with oxalyl chloride (30.8 mL, 0.353 mol), refluxed for 3 hours, cooled, and concentrated in vacuo to obtain the title product as an orange solid which is identified by NMR spectral analysis.

후처리

  1. temperaturerefluxed for 3 hours
  2. temperaturecooled
  3. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-77741e50a88d4d9fb0e0a54fbf5403c2
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06706663B2

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