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Sodium hydride → 6,7-Dimethoxy-1-(3-methylsulfanyl-benzoyl)-isoquinoline-4-carbonitrile

HRID 1833240
ノート
印刷プレビュー

反応式

HRID 1833240 の反応式
Br[C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[C:5]([C:16]#[N:17])=[CH:4][N:3]=1.[CH3:18][S:19][C:20]1[CH:21]=[C:22]([CH:25]=[CH:26][CH:27]=1)[CH:23]=[O:24].[I-].C[NH+]1C=CN(C)C1.[H-].[Na+]>CN(C)C=O.C(OCC)(=O)C.CCCCCC.O>[CH3:15][O:14][C:8]1[CH:7]=[C:6]2[C:11](=[CH:10][C:9]=1[O:12][CH3:13])[C:2]([C:23](=[O:24])[C:22]1[CH:25]=[CH:26][CH:27]=[C:20]([S:19][CH3:18])[CH:21]=1)=[N:3][CH:4]=[C:5]2[C:16]#[N:17]
参加物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 127211713-(Methylsulfanyl)benzaldehydeHCID 220483501-Bromo-6,7-dimethoxyisoquinoline-4-carbonitrileHCID 236182761,3-Dimethyl-1H-imidazolium iodide

生成物 1

HCID 220483856,7-Dimethoxy-1-(3-methylsulfanyl-benzoyl)-isoquinoline-4-carbonitrile収率 57%

試薬・触媒・溶媒 3

HCID 962
Water
溶媒
HCID 6228Dimethylformamide溶媒
HCID 21226206Ethyl acetate hexane溶媒

実験手順

To a stirred solution of 1-bromo-6,7-dimethoxy-isoquinoline-4-carbonitrile (100 mg, 0.34 mmol), 3-methylsulfanyl-benzaldehyde (104 g, 0.68 mmol) and 1,3-dimethyl-1H-imidazolium iodide (153 mg, 0.68 mmol) in N,N-dimethylformamide (3 mL) was added sodium hydride (27.3 mg, 0.68 mmol). The mixture turned black instantly. The reaction mixture was stirred at room temperature for 1 h. Water was added and the aqueous phase was extracted with dichloromethane (3×20 mL). The combined extracts were washed with saturated sodium chloride solution (20 mL), dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. Flash chromatography (Merck Silica gel 60, 70–230 mesh, 20% ethyl acetate/hexane) afforded 6,7-dimethoxy-1-(3-methylsulfanyl-benzoyl)-isoquinoline-4-carbonitrile (70 mg, 57% yield) as a colorless oil.

後処理

  1. extractionthe aqueous phase was extracted with dichloromethane (3×20 mL)
  2. washThe combined extracts were washed with saturated sodium chloride solution (20 mL)
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-12534dc908594ef2922d0d36e08f2aea
出典データセット
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07067529B2

反応ノート

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