Nitric Acid → HCID 68584619、化合物

HRID 17530

反応式

HRID 17530 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[F:10])[C:5]#[N:6].[N+:11]([O-])([OH:13])=[O:12]>S(=O)(=O)(O)O>[Br:1][C:2]1[C:9]([F:10])=[CH:8][C:7]([N+:11]([O-:13])=[O:12])=[C:4]([CH:3]=1)[C:5]#[N:6]

参加物

4

反応物 2

HCID 944Nitric AcidHCID 1235793-Bromo-4-fluorobenzonitrile

生成物 1

HCID 68584619HCID 68584619、化合物収率 48%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

3-Bromo-4-fluorobenzonitrile (25 g, 0.125 mol) was dissolved in concentrated sulfuric acid (200 ml), and at 0° C., fuming nitric acid was dropwise added at 0° C., taking 1 hour. After stirred for 30 minutes at the same temperature, this was heated up to room temperature, taking 1.5 hours. This was gradually poured into ice. The formed precipitate was collected by filtration with washing with water, and dried under reduced pressure. The collected yellow powder was fractionated with chloroform and aqueous 1 M sodium hydroxide solution. The organic layer was washed with saturated brine, then dried over anhydrous sodium sulfate. The solvent was evaporated away, and the resulting residue was well dried under reduced pressure to obtain the entitled compound (14.7 g, 48%) as a yellow powder.

後処理

  1. customat 0° C.
  2. additionwas dropwise added at 0° C.
  3. waittaking 1.5 hours
  4. additionThis was gradually poured into ice
  5. filtrationThe formed precipitate was collected by filtration
  6. washwith washing with water
  7. customdried under reduced pressure
  8. washThe organic layer was washed with saturated brine
  9. dry with materialdried over anhydrous sodium sulfate
  10. customThe solvent was evaporated away
  11. customthe resulting residue was well dried under reduced pressure

出典と根拠

ORDレコード
ord-3e240567bde4449c8214003cc724eb2f
出典データセット
uspto-grants-2010_06
特許番号
US07737166B2

関連ノート

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