Nitric Acid → 2,4-Difluoro-5-nitrobenzoic acid

HRID 6863

反応式

HRID 6863 の反応式
[F:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[N+:12]([O-])([OH:14])=[O:13]>S(=O)(=O)(O)O>[F: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]([OH:6])=[O:5]

参加物

4

反応物 2

HCID 944Nitric AcidHCID 741022,4-Difluorobenzoic acid

生成物 1

HCID 27828222,4-Difluoro-5-nitrobenzoic acid収率 98%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

To a suspension of 2,4-difluorobenzoic acid (9.985 g, 63.2 mmol) in concentrated sulfuric acid (30 mL) at 0° C. was added fuming nitric acid (30 mL) over 30 min. The mixture was allowed to warm to RT and stirred for an additional 16 h. The homogeneous mixture was poured onto ice and extracted with ethyl acetate. The organic extract was washed with water, dried and concentrated in vacuo to afford 2,4-difluoro-5-nitrobenzoic acid (12.56 gm, 98%) as pale yellow solid.

後処理

  1. additionThe homogeneous mixture was poured onto ice
  2. extractionextracted with ethyl acetate
  3. extractionThe organic extract
  4. washwas washed with water
  5. customdried
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-8e536b4f293e4a9abaef797cf8c29f57
出典データセット
uspto-grants-2006_08
特許番号
US07084160B2

関連ノート

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