Hydrochloric Acid → 3-Acetyl-5-(trifluoromethyl)benzonitrile

HRID 906336ノート

反応式

HRID 906336 の反応式
[C:1]([C:3]1[CH:4]=[C:5]([CH:12]=[C:13]([C:15]([F:18])([F:17])[F:16])[CH:14]=1)[C:6](N(OC)C)=[O:7])#[N:2].[CH3:19][Mg]Br.Cl>O1CCCC1>[C:6]([C:5]1[CH:4]=[C:3]([CH:14]=[C:13]([C:15]([F:18])([F:17])[F:16])[CH:12]=1)[C:1]#[N:2])(=[O:7])[CH3:19]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 866284333-cyano-N-methoxy-N-methyl-5-(trifluoromethyl)benzamideHCID 178418573HCID 178418573、化合物

生成物 1

HCID 673907473-Acetyl-5-(trifluoromethyl)benzonitrile収率 103.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 3-cyano-N-methoxy-N-methyl-5-(trifluoromethyl)benzamide (196 mg, 0.76 mmol) in anhydrous tetrahydrofuran (2 mL) was added with methylmagnesium bromide (0.96 M solution in ether, 0.95 mL, 0.91 mmol) with stirring on an ice bath, and the mixture was stirred at room temperature for 15 minutes. The reaction mixture was added with 1 M hydrochloric acid, and the mixture was extracted with ethyl acetate. Then, the organic layer was washed with saturated brine, dried over anhydrous sodium sulfate, and then concentrated under reduced pressure to obtain 3-acetyl-5-(trifluoromethyl)benzonitrile (167.4 mg, 100%) as pale yellow oil.

後処理

  1. stirringthe mixture was stirred at room temperature for 15 minutes
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThen, the organic layer was washed with saturated brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-ae4bb7185c7042d987067915f8d89488
出典データセット
uspto-grants-2011_09
特許番号
US08012989B2

反応ノート

読み込み中…