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Sodium hydride → N,N-dimethyl-2-((4-methylpyridin-3-yl)amino)benzamide

HRID 1801498
ノート
印刷プレビュー

反応式

HRID 1801498 の反応式
[NH2:1][C:2]1[CH:12]=[CH:11][CH:10]=[CH:9][C:3]=1[C:4]([N:6]([CH3:8])[CH3:7])=[O:5].Cl[C:14]1[CH:15]=[N:16][CH:17]=[CH:18][C:19]=1[CH3:20].C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1.[H-].[Na+]>O1CCOCC1.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.ClCCl>[CH3:7][N:6]([CH3:8])[C:4](=[O:5])[C:3]1[CH:9]=[CH:10][CH:11]=[CH:12][C:2]=1[NH:1][C:14]1[CH:15]=[N:16][CH:17]=[CH:18][C:19]=1[CH3:20]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 24758Sodium hydrideHCID 634876Binap, (A+-)-HCID 27629253-Chloro-4-methylpyridineHCID 47781752-Amino-N,N-dimethylbenzamide

生成物 1

HCID 59506321N,N-dimethyl-2-((4-methylpyridin-3-yl)amino)benzamide収率 26%

試薬・触媒・溶媒 3

HCID 167845
palladium(II) acetate
触媒
HCID 6344Dichloromethane溶媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

To a mixture of 2-amino-N,N-dimethylbenzamide (1.3 g, 6.77 mmol), 3-chloro-4-methylpyridine (0.745 mL, 6.77 mmol), Palladium acetate (0.150 g) and BINAP (0.60 g) in 1,4-dioxane (10 mL) was added NaH (0.677 g, 16.93 mmol) and the resulting mixture was heated at 100° C. for 2 hours. The solvent was removed under reduced pressure. The residue obtained was taken into dichloromethane (50 mL) and filtered through celite. The filtrate was washed with water (50 mL), dried over sodium sulfate and concentrated under reduced pressure. The crude product was purified using flash column chromatography (SiO2) to provide 0.450 g of the desired product as a dark oil.

後処理

  1. customThe solvent was removed under reduced pressure
  2. customThe residue obtained
  3. filtrationfiltered through celite
  4. washThe filtrate was washed with water (50 mL)
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe crude product was purified

出典と根拠

ORDレコード
ord-3c4ae5cdd3ce4122b77079efb1097140
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08349827B2

反応ノート

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