Sulfuric Acid → 2,3-Difluoro-5-nitrobenzoic acid

HRID 2171223노트

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HRID 2171223 반응식
[N+:1]([O-:4])([O-])=[O:2].[Na+].S(=O)(=O)(O)O.[F:11][C:12]1[C:20]([F:21])=[CH:19][CH:18]=[CH:17][C:13]=1[C:14]([OH:16])=[O:15]>>[F:11][C:12]1[C:20]([F:21])=[CH:19][C:18]([N+:1]([O-:4])=[O:2])=[CH:17][C:13]=1[C:14]([OH:16])=[O:15]

참가 물질

4

반응물 3

HCID 1118Sulfuric AcidHCID 24268Sodium NitrateHCID 3705902,3-Difluorobenzoic acid

생성물 1

HCID 545937902,3-Difluoro-5-nitrobenzoic acid수율 79.3%

실험 절차

Sodium nitrate (1.7 g) was added to a concentrated sulfuric acid (7 ml) solution containing 2,3-difluorobenzoic acid (1.58 g), followed by stirring at room temperature for 0.5 hours. The reaction solution was poured into ice water, followed by extraction with ethyl acetate. The organic layers were dried over anhydrous sodium sulfate. The solvent was distilled away under reduced pressure, the obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=1:0 to 4:1). A light yellow solid of 2,3-difluoro-5-nitrobenzoic acid (1.61 g) was thus obtained.

후처리

  1. extractionfollowed by extraction with ethyl acetate
  2. dry with materialThe organic layers were dried over anhydrous sodium sulfate
  3. distillationThe solvent was distilled away under reduced pressure
  4. customthe obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=1:0 to 4:1)

출처 및 근거

ORD 기록
ord-740305b99cd64764a2fa43807f540aea
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09051310B2

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