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Diethyl Ether → [(2,4-Dimethoxyphenyl)methyl](methyl)amine

HRID 1644631
ノート
印刷プレビュー

反応式

HRID 1644631 の反応式
[CH3:1][O:2][C:3]1[CH:12]=[C:11]([O:13][CH3:14])[CH:10]=[CH:9][C:4]=1[CH2:5][NH:6][CH:7]=O.[AlH4-].[Li+].CCOCC>>[CH3:1][O:2][C:3]1[CH:12]=[C:11]([O:13][CH3:14])[CH:10]=[CH:9][C:4]=1[CH2:5][NH:6][CH3:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 3283Diethyl EtherHCID 28112Lithium aluminum hydrideHCID 21465904N-(2,4-Dimethoxy-benzyl)-formamide

生成物 1

HCID 2416536[(2,4-Dimethoxyphenyl)methyl](methyl)amine収率 82%

実験手順

N-(2,4-Dimethoxy-benzyl)-formamide (0.50 g, 2.6 mmol) was added slowly to a suspension of the lithium tetrahydroaluminate (0.19 g, 5.1 mmol) in ether (30 mL, 200 mmol) at −78° C. The reaction mixture was warmed slowly to rt and stirred at rt under an atmosphere of Argon over night. The reaction was quenched at 0° C. by the sequential addition of 0.19 ml of H2O, 0.19 ml of 15% aq NaOH solution, and 0.57 ml of the H2O. The inorganic solids were removed by filtration and washed with ether. The ether filtrate was washed with water and brine, dried over Na2SO4. Evaporation of the solvent gave the product as a pale yellow oil (0.38 g, 82%).

後処理

  1. customThe reaction was quenched at 0° C. by the sequential addition of 0.19 ml of H2O, 0.19 ml of 15% aq NaOH solution, and 0.57 ml of the H2O
  2. customThe inorganic solids were removed by filtration
  3. washwashed with ether
  4. washThe ether filtrate was washed with water and brine
  5. dry with materialdried over Na2SO4
  6. customEvaporation of the solvent

出典と根拠

ORDレコード
ord-cce8caa23ce247cdbcff8a4bea972154
出典データセット
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08124610B2

反応ノート

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