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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Sodium Iodide → HCID 21409856、化合物

HRID 2072009
ノート
印刷プレビュー

反応式

HRID 2072009 の反応式
[CH3:1][NH:2][C:3]([CH3:15])([CH3:14])[CH2:4][NH:5][C:6](=[O:13])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.BrC[CH:18]=[C:19]([CH3:21])[CH3:20].[C:22](=O)([O-])[O-].[Na+].[Na+].[I-].[Na+]>CC(CC)=O>[CH3:14][C:3]([N:2]([CH3:22])[CH2:1][CH:18]=[C:19]([CH3:21])[CH3:20])([CH3:15])[CH2:4][NH:5][C:6](=[O:13])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 5238Sodium IodideHCID 10340Sodium CarbonateHCID 700922-Butene, 1-bromo-3-methyl-HCID 21409819N-[2-Methylamino-2-methylpropyl]benzamide

生成物 1

HCID 21409856HCID 21409856、化合物収率 84.1%

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone
溶媒
2 回

実験手順

A solution of N[2-methylamino-2-methylpropyl] benzamide (1 g., 0.0052 mole) in methylethyl ketone (MEK) (25 ml.) was added to a solution of 1-bromo-3-methyl-but-2-ene (0.78 g., 0.0052 mole) in MEK (40 ml.) containing sodium carbonate (0.55 g., 0.0052 mole) and a few crystals of sodium iodide. The mixture was heated under reflux for 30 hrs. The inorganic solids were filtered off and the filtrant concentrated by evaporation under reduced pressure to give a liquid residue. This was loaded onto an alumina column and eluted with ethyl acetate. Fractions (25 mls) were collected and concentrated to give N[2-methyl-2[methyl(3-methyl-2-butenyl)amino]propyl]benzamide (1.2 g.).

後処理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 30 hrs
  3. filtrationThe inorganic solids were filtered off
  4. concentrationthe filtrant concentrated by evaporation under reduced pressure
  5. customto give a liquid residue
  6. washeluted with ethyl acetate
  7. customFractions (25 mls) were collected
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-a410465cd8334cfab880f8ce9c025d67
出典データセット
uspto-grants-1977_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04049663

反応ノート

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