Nitric Acid → HCID 15278570、化合物

HRID 1440129ノート

反応式

HRID 1440129 の反応式
[Br:1][C:2]1[C:3]([C:12]2[CH:17]=[C:16]([F:18])[CH:15]=[CH:14][C:13]=2[F:19])=[N:4][N:5]([CH3:11])[C:6]=1[C:7]([F:10])([F:9])[F:8].[N+:20]([O-])([OH:22])=[O:21]>>[Br:1][C:2]1[C:3]([C:12]2[CH:17]=[C:16]([F:18])[C:15]([N+:20]([O-:22])=[O:21])=[CH:14][C:13]=2[F:19])=[N:4][N:5]([CH3:11])[C:6]=1[C:7]([F:8])([F:9])[F:10]

参加物

3

反応物 2

HCID 944Nitric AcidHCID 110569594-bromo-3-(2,5-difluorophenyl)-1-methyl-5-(trifluoromethyl)-1H-pyrazole

生成物 1

HCID 15278570HCID 15278570、化合物収率 55%

反応条件

温度
28 °C

実験手順

At 15° C., 9.5 g (0.03 mole) 4-bromo-3-(2,5-difluorophenyl)-1-methyl-5-(trifluoromethyl)-1H-pyrazole was slowly added to 100 mL of fuming nitric acid. The reaction warmed to 28° C. over a period of 20 minutes. The reaction mixture was stirred at 30° C. for 4 hours. The mixture was poured into 500 mL of ice. After stirring for 1 hour, the slurry was extracted 3 times with methylene chloride. The methylene chloride extracts were washed with water, dried over anhydrous MgSO4, and concentrated in vacuo. The residue was purified chromatographically using 10% ethyl acetate in hexane as the eluent to give 5.84 g (55%) of 4-bromo-3-(2,5-difluoro-4-nitrophenyl)-1-methyl-5-(trifluoromethyl)-1H-pyrazole as a white solid, mp 45.5° C.

後処理

  1. stirringAfter stirring for 1 hour
  2. extractionthe slurry was extracted 3 times with methylene chloride
  3. washThe methylene chloride extracts were washed with water
  4. dry with materialdried over anhydrous MgSO4
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified chromatographically

出典と根拠

ORDレコード
ord-9e62cb2f053b4acba739abc691dc6004
出典データセット
uspto-grants-1996_03
特許番号
US05496956

反応ノート

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