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

HRID 6863

반응식

HRID 6863 반응식
[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]

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 741022,4-Difluorobenzoic acid

생성물 1

HCID 27828222,4-Difluoro-5-nitrobenzoic acid수율 98%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8e536b4f293e4a9abaef797cf8c29f57
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07084160B2

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