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

HRID 1442519노트

반응식

HRID 1442519 반응식
[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]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 866284333-cyano-N-methoxy-N-methyl-5-(trifluoromethyl)benzamideHCID 178418573HCID 178418573, 화합물

생성물 1

HCID 673907473-Acetyl-5-(trifluoromethyl)benzonitrile수율 100%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 3-cyano-N-methoxy-N-methyl-5-(trifluoromethyl)benzamide (196 mg, 0.76 mmol) in anhydrous tetrahydrofuran (2 mL) stirred on an ice bath was added methylmagnesium bromide (0.96 M solution in ether, 0.95 mL, 0.91 mmol), and the mixture was stirred at room temperature for 15 minutes. The reaction mixture was added with 1 M hydrochloric acid, and extracted with ethyl acetate, and 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 (162 mg, 100%) as a pale yellow oil.

후처리

  1. extractionextracted with ethyl acetate
  2. washthe organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-936d8c76b53d43078b092efacbe6cff3
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07659271B2

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