3-Bromobenzyl bromide → Benzenemethanamine, 3-bromo-N-ethyl-

HRID 2403565ノート

反応式

HRID 2403565 の反応式
[CH2:1]([NH2:3])[CH3:2].CO.[Br:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([CH2:13]Br)[CH:8]=1>>[Br:6][C:7]1[CH:8]=[C:9]([CH:10]=[CH:11][CH:12]=1)[CH2:13][NH:3][CH2:1][CH3:2]

参加物

3

反応物 2

HCID 699793-Bromobenzyl bromideHCID 86635283HCID 86635283、化合物

生成物 1

HCID 457589Benzenemethanamine, 3-bromo-N-ethyl-収率 71.2%

実験手順

To 80% ethylamine/MeOH (1.1 g) was added 1-bromo-3-(bromomethyl)benzene (1 g) in five divided portions at room temperature, followed by stirring at room temperature overnight. The reaction mixture was concentrated under reduced pressure, and the obtained residue was subjected to liquid separation with chloroform and a saturated aqueous sodium hydrogen carbonate solution. The organic layer was separated, and then the aqueous layer was extracted with CHCl3 again. These organic layers were combined, dried over Na2SO4, and then concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (NH silica, 3% MeOH/CHCl3) to obtain N-(3-bromobenzyl)ethanamine (610 mg) as a colorless oil.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customthe obtained residue was subjected to liquid separation with chloroform
  3. customThe organic layer was separated
  4. extractionthe aqueous layer was extracted with CHCl3 again
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated under reduced pressure
  7. customThe obtained residue was purified by silica gel column chromatography (NH silica, 3% MeOH/CHCl3)

出典と根拠

ORDレコード
ord-eeb8e6bc287847d8bc7ed3e85461c726
出典データセット
uspto-grants-2014_08
特許番号
US08802679B2

反応ノート

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