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5-iodo-4-[(4-methyl-1H-indol-5-yl)amino]nicotinonitrile → 5-(5-formyl-1-benzofuran-2-yl)-4-[(4-methyl-1H-indol-5-yl)amino]nicotinonitrile

HRID 506193
ノート
印刷プレビュー

反応式

HRID 506193 の反応式
I[C:2]1[CH:3]=[N:4][CH:5]=[C:6]([C:9]=1[NH:10][C:11]1[C:12]([CH3:20])=[C:13]2[C:17](=[CH:18][CH:19]=1)[NH:16][CH:15]=[CH:14]2)[C:7]#[N:8].C([Sn](CCCC)(CCCC)[C:26]1[O:27][C:28]2[CH:34]=[CH:33][C:32]([CH:35]=[O:36])=[CH:31][C:29]=2[CH:30]=1)CCC>CN(C=O)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH:35]([C:32]1[CH:33]=[CH:34][C:28]2[O:27][C:26]([C:2]3[CH:3]=[N:4][CH:5]=[C:6]([C:9]=3[NH:10][C:11]3[C:12]([CH3:20])=[C:13]4[C:17](=[CH:18][CH:19]=3)[NH:16][CH:15]=[CH:14]4)[C:7]#[N:8])=[CH:30][C:29]=2[CH:31]=1)=[O:36]
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

5

反応物 2

HCID 684438315-iodo-4-[(4-methyl-1H-indol-5-yl)amino]nicotinonitrileHCID 866168342-(Tributylstannyl)-1-benzofuran-5-carbaldehyde

生成物 1

HCID 866168355-(5-formyl-1-benzofuran-2-yl)-4-[(4-methyl-1H-indol-5-yl)amino]nicotinonitrile収率 76.1%

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒
HCID 6228
Dimethylformamide
溶媒

反応条件

温度
120 °C

実験手順

A mixture of 5-iodo-4-[(4-methyl-1H-indol-5-yl)amino]nicotinonitrile (2.5 g, 6.7 mmol), 2-(tributylstannyl)-1-benzofuran-5-carbaldehyde (4.35 g, 10 mmol), and tetrakis(triphenylphosphine)palladium(0) (0.38 g, 0.34 mmol) in DMF (25 mL) was heated at 120° C. for 1 h. The reaction mixture was cooled to room temperature and partitioned between ethyl acetate and water, resulting in a suspension. The insoluble material was removed by filtration and the residue was washed thoroughly with ethyl acetate. The organic layer (from filtrate) was washed with water twice and brine, dried over sodium sulfate, and concentrated and the residue was purified by column chromatography (ethyl acetate/hexane, 1:1) to give 2.0 g (76%) of 5-(5-formyl-1-benzofuran-2-yl)-4-[(4-methyl-1H-indol-5-yl)amino]nicotinonitrile as a yellow solid. HPLC retention time: 10.7 min.(h); MS: 393.2 (M+H); melting point: 235-237° C.; and HRMS: 393.13484.

後処理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. custompartitioned between ethyl acetate and water
  3. customresulting in a suspension
  4. customThe insoluble material was removed by filtration
  5. washthe residue was washed thoroughly with ethyl acetate
  6. washThe organic layer (from filtrate) was washed with water twice
  7. dry with materialbrine, dried over sodium sulfate
  8. concentrationconcentrated
  9. customthe residue was purified by column chromatography (ethyl acetate/hexane, 1:1)

出典と根拠

ORDレコード
ord-3835316e2c3741ae8981c9e2bfb8ef04
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07781591B2

反応ノート

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