Dimethylformamide → 2,3-Difluoro-5-(trifluoromethyl)benzonitrile

HRID 1614418노트

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HRID 1614418 반응식
S(Cl)(Cl)=O.[F:5][C:6]1[C:14]([F:15])=[CH:13][C:12]([C:16]([F:19])([F:18])[F:17])=[CH:11][C:7]=1[C:8]([NH2:10])=O.CN(C)C=O.C(=O)([O-])[O-].[K+].[K+]>CCCCC>[F:5][C:6]1[C:14]([F:15])=[CH:13][C:12]([C:16]([F:19])([F:17])[F:18])=[CH:11][C:7]=1[C:8]#[N:10]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 24386Thionyl ChlorideHCID 19773828HCID 19773828, 화합물

생성물 1

HCID 190908472,3-Difluoro-5-(trifluoromethyl)benzonitrile수율 56%

시약·촉매·용매 1

HCID 8003Pentane용매

실험 절차

Thionyl chloride, 6.0 g (50 mmol) was added to a slurry of 4.0 g (18 mmol) 2,3-difluoro-5-(trifluoromethyl)benzamide and 15 mL dimethylformamide at 0° C. After stirring for 1 hour, the reaction mixture was diluted with 25 mL pentane and neutralized by dropwise addition of a saturated potassium carbonate solution and filtered. The pentane solution was dried and distilled to yield 2,3-difluoro-5-(trifluoromethyl) benzonitrile in 56% yield, bp 65°-70° C./20 mm Hg.

후처리

  1. filtrationfiltered
  2. dry with materialThe pentane solution was dried
  3. distillationdistilled

출처 및 근거

ORD 기록
ord-c908633bde49442cb0736bc839a25c86
출처 데이터셋
uspto-grants-1993_03
특허 번호
US05196593

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