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Methyl iodide → 2-(4-acetyl-phenylazo)-2-(2,3,3-trimethyl-3,4-dihydro-2H-isoquinoline-1-ylidene)-acetamide

HRID 333634
ノート
印刷プレビュー

反応式

HRID 333634 の反応式
[C:1]([C:4]1[CH:9]=[CH:8][C:7]([N:10]=[N:11][C:12](=[C:16]2[C:25]3[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=3)[CH2:19][C:18]([CH3:27])([CH3:26])[NH:17]2)[C:13]([NH2:15])=[O:14])=[CH:6][CH:5]=1)(=[O:3])[CH3:2].[C:28](=O)([O-])[O-].[Na+].[Na+].CI>C(#N)C>[C:1]([C:4]1[CH:5]=[CH:6][C:7]([N:10]=[N:11][C:12](=[C:16]2[C:25]3[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=3)[CH2:19][C:18]([CH3:27])([CH3:26])[N:17]2[CH3:28])[C:13]([NH2:15])=[O:14])=[CH:8][CH:9]=1)(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 10340Sodium CarbonateHCID 178466770HCID 178466770、化合物

生成物 1

HCID 729756002-(4-acetyl-phenylazo)-2-(2,3,3-trimethyl-3,4-dihydro-2H-isoquinoline-1-ylidene)-acetamide

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

2-(4-acetyl-phenylazo)-2-(3,3-dimethyl-3,4-dihydro-2H-isoquinoline-1-ylidene) acetamide (Asinex Corp., Russia) and sodium carbonate are added to acetonitrile, and an acetonitrile solution of methyl iodide is slowly dropped and refluxed. The refluxed product is cooled to room temperature and, then, the solvent is removed by reducing a pressure; the residue is dissolved in dichloromethane and washed with distilled water. Thereafter, the product is dried with anhydrous sodium sulfate and filtered and, then, the solvent is removed by reducing the pressure. The residue containing the reaction product is purified by column chromatography to obtain the title compound.

後処理

  1. temperaturerefluxed
  2. customthe solvent is removed
  3. dissolutionthe residue is dissolved in dichloromethane
  4. washwashed with distilled water
  5. dry with materialThereafter, the product is dried with anhydrous sodium sulfate
  6. filtrationfiltered
  7. customthe solvent is removed
  8. additionThe residue containing the reaction product
  9. customis purified by column chromatography

出典と根拠

ORDレコード
ord-56621459cfc44fc2a624ea0d050e8b77
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08883504B2

反応ノート

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