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Nitric Acid → N-(2-fluoro-4-nitro-5-carboxyphenyl)-2,3-dimethylmaleic acid imide

HRID 1651480
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HRID 1651480 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([OH:10])=[O:9])=[CH:4][C:3]=1[N:11]1[C:15](=[O:16])[C:14]([CH3:17])=[C:13]([CH3:18])[C:12]1=[O:19].[N+:20]([O-])([OH:22])=[O:21]>S(=O)(=O)(O)O>[F:1][C:2]1[CH:7]=[C:6]([N+:20]([O-:22])=[O:21])[C:5]([C:8]([OH:10])=[O:9])=[CH:4][C:3]=1[N:11]1[C:15](=[O:16])[C:14]([CH3:17])=[C:13]([CH3:18])[C:12]1=[O:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 17802078N-(2-fluoro-5-carboxyphenyl)-2,3-dimethylmaleic acid imide

생성물 1

HCID 54493468N-(2-fluoro-4-nitro-5-carboxyphenyl)-2,3-dimethylmaleic acid imide

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

26.3 g of N-(2-fluoro-5-carboxyphenyl)-2,3-dimethylmaleic acid imide are introduced in portions, at 5°, into 230 ml of 96% sulphuric acid. There is then added dropwise to this mixture, while stirring vigorously at the same temperature, 5 ml of 100% nitric acid. The whole is further stirred overnight at room temperature and then poured onto ice. The product which precipitates is filtered with suction, washed with water, dried and recrystallised from acetonitrile. 28 g of N-(2-fluoro-5-carboxy-4-nitrophenyl)-2,3-dimethylmaleic acid imide which has a melting point of 264°-265° is thus obtained.

후처리

  1. additionThere is then added dropwise to this mixture
  2. additionpoured onto ice
  3. customThe product which precipitates
  4. filtrationis filtered with suction
  5. washwashed with water
  6. customdried
  7. customrecrystallised from acetonitrile
  8. customis thus obtained

출처 및 근거

ORD 기록
ord-d8c70f73e1184262bfd31690282f997a
출처 데이터셋
uspto-grants-1990_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04929272

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