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2,4-Dimethylaniline → Aniline

HRID 598056
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HRID 598056 반응식
Br[C:2]1[C:3](=[O:12])[N:4]([CH3:11])[CH:5]=[C:6]([N+:8]([O-:10])=[O:9])[CH:7]=1.[CH3:13][C:14]1[CH:20]=[C:19]([CH3:21])[CH:18]=[CH:17][C:15]=1[NH2:16].C1(P(C2C=CC=CC=2)C2C=CC3C(=CC=CC=3)C=2C2C3C(=CC=CC=3)C=CC=2P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.CC(C)([O-])C.[Na+]>C1(C)C=CC=CC=1.C(OCC)(=O)C.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[CH3:13][C:14]1[CH:20]=[C:19]([CH3:21])[CH:18]=[CH:17][C:15]=1[NH:16][C:2]1[C:3](=[O:12])[N:4]([CH3:11])[CH:5]=[C:6]([N+:8]([O-:10])=[O:9])[CH:7]=1.[NH2:16][C:15]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:14]=1
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참가 물질

9

반응물 4

HCID 72502,4-DimethylanilineHCID 634876Binap, (A+-)-HCID 23676156Sodium t-butoxideHCID 672674813-Bromo-1-methyl-5-nitro-2(1H)-pyridinone

생성물 2

HCID 6115AnilineHCID 672679503-[(2,4-Dimethylphenyl)amino]-1-methyl-5-nitropyridin-2(1H)-one

시약·촉매·용매 3

HCID 9811564Bis(dibenzylideneacetone)palladium촉매HCID 1140Toluene용매HCID 8857Ethyl Acetate용매

반응 조건

온도
95 °C

실험 절차

To a solution containing 0.60 g (2.57 mmol) of 3-bromo-1-methyl-5-nitropyridin-2(1H)-one in 120 ml of toluene under a nitrogen atmosphere was added 0.64 ml (5.15 mmol) of 2,4-dimethylaniline, 1.61 g (2.57 mmol) of rac-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (racemic BINAP), 0.37 g (3.85 mmol) of sodium t-butoxide and 1.20 g (1.31 mmol) of tris(dibenzylideneacetone)dipalladium (0). The reaction was heated to 95° C. overnight. The reaction was cooled to room temperature, diluted with ethyl acetate and washed with saturated sodium bicarbonate. The organic phase was dried over magnesium sulfate. Filtration, removal of solvent and purification of the residue via biotage eluting with 60% ethyl acetate/hexanes gave the desired product with some starting aniline. The material was triturated with hexanes and the solids filtered and dried to afford 0.154 g (21.9%) of product.

후처리

  1. temperatureThe reaction was cooled to room temperature
  2. washwashed with saturated sodium bicarbonate
  3. dry with materialThe organic phase was dried over magnesium sulfate
  4. filtrationFiltration, removal of solvent and purification of the residue via biotage
  5. washeluting with 60% ethyl acetate/hexanes

출처 및 근거

ORD 기록
ord-6f11ef843c1843bf979f4d549fc34825
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07897607B2

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