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

HRID 2171223ノート

反応式

HRID 2171223 の反応式
[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]

参加物

4

反応物 3

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

生成物 1

HCID 545937902,3-Difluoro-5-nitrobenzoic acid収率 79.3%

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-740305b99cd64764a2fa43807f540aea
出典データセット
uspto-grants-2015_06
特許番号
US09051310B2

反応ノート

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