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Cesium carbonate → HCID 59405009、化合物

HRID 1672201
ノート
印刷プレビュー

反応式

HRID 1672201 の反応式
Cl[C:2]1[CH:3]=[C:4]([NH:12][C:13]2[N:14]=[CH:15][C:16]3[CH2:17][C:18](=[O:32])[NH:19][C:20]4[CH:27]=[C:26]([C:28]([F:31])([F:30])[F:29])[CH:25]=[CH:24][C:21]=4[C:22]=3[N:23]=2)[C:5]([C:8]([F:11])([F:10])[F:9])=[N:6][CH:7]=1.[CH2:33]([N:36]([CH3:38])[CH3:37])[C:34]#[CH:35].C(=O)([O-])[O-].[Cs+].[Cs+].CC(C1C=C(C(C)C)C(C2C=CC=CC=2P(C2CCCCC2)C2CCCCC2)=C(C(C)C)C=1)C>CN(C=O)C.CC#N.CC#N.Cl[Pd]Cl>[CH3:37][N:36]([CH3:38])[CH2:33][C:34]#[C:35][C:2]1[CH:3]=[C:4]([NH:12][C:13]2[N:14]=[CH:15][C:16]3[CH2:17][C:18](=[O:32])[NH:19][C:20]4[CH:27]=[C:26]([C:28]([F:31])([F:29])[F:30])[CH:25]=[CH:24][C:21]=4[C:22]=3[N:23]=2)[C:5]([C:8]([F:11])([F:9])[F:10])=[N:6][CH:7]=1
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

7

反応物 4

HCID 10796Cesium carbonateHCID 81643N,N-DimethylpropargylamineHCID 111557942-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenylHCID 59405022HCID 59405022、化合物

生成物 1

HCID 59405009HCID 59405009、化合物収率 67.3%

試薬・触媒・溶媒 2

HCID 6093782
Bis(acetonitrile)dichloropalladium
触媒
HCID 6228Dimethylformamide溶媒

反応条件

温度
150 °C

実験手順

A mixture of 2-{[5-chloro-2-(trifluoromethyl)pyridin-3-yl]amino}-9-(trifluoromethyl)-5,7-dihydro-6H-pyrimido[5,4-d][1]benzazepin-6-one (0.058 g, 0.12 mmol), propargyl(dimethylamine) (0.016 mL, 0.15 mmol) and cesium carbonate (0.080 g, 0.25 mmol) in DMF (0.60 ml) was degassed for 15 min with argon. To the suspension were added bis(acetonitrile)palladium(II)chloride (0,0020 g, 0.0061 mmol) and Xphos (0.0076 g, 0.016 mmol). The suspension was purged three times with nitrogen and was then allowed to stir at 150° C. for 48 h. The mixture was filtered through celite and the filtrate was concentrated. The residue was purified by column chromatography to give 2-{[5-[3-(dimethylamino)prop-1-yn-1-yl]-2-(trifluoromethyl)pyridin-3-yl]amino}-9-(trifluoromethyl)-5,7-dihydro-6H-pyrimido[5,4-d][1]benzazepin-6-one (0.042g, 66%) as a solid.

後処理

  1. customwas degassed for 15 min with argon
  2. customThe suspension was purged three times with nitrogen
  3. filtrationThe mixture was filtered through celite
  4. concentrationthe filtrate was concentrated
  5. customThe residue was purified by column chromatography

出典と根拠

ORDレコード
ord-bfd260e07d5e4d928daad08ee5bf9812
出典データセット
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07998952B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート