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Sodium Hydroxide → 4-Trifluoromethylnicotinamide

HRID 1744272
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HRID 1744272 반응식
[F:1][C:2]([F:13])([F:12])[C:3](=O)[CH:4]=[CH:5][NH:6][CH:7]=[CH:8][C:9]#[N:10].[OH-].[Na+].CCCCCC.CC(C)=[O:24]>CO>[F:1][C:2]([F:13])([F:12])[C:3]1[C:8]([C:9]([NH2:10])=[O:24])=[CH:7][N:6]=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 21880519Acetone hexaneHCID 731022503-[(4,4,4-Trifluoro-3-oxo-1-butenyl)amino]-2-propenenitrile

생성물 1

HCID 27826434-Trifluoromethylnicotinamide수율 65.6%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

3-[(4,4,4-Trifluoro-3-oxo-1-butenyl)amino]-2propenenitrile (a mixture of IIa and IIb; 1.90 g, 10 mmol) was dissolved in methanol (15 ml), and sodium hydroxide (600 mg, 15 mmol) was added. The mixture was heated under reflux for 6 hours. The reaction mixture was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (a eluting solvent: hexane/acetone=1/1) to obtain 1.25 g (yield 65.6%) of the title compound.

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 6 hours
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. customThe resulting residue was purified by silica gel column chromatography (a eluting solvent

출처 및 근거

ORD 기록
ord-5d615dc0d391490cb063e8c10c01152d
출처 데이터셋
uspto-grants-2006_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07015236B2

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