Aluminium lithium hydride → 1-[(1-Aminopropan-2-YL)oxy]-2-methoxybenzene

HRID 1596782ノート

反応式

HRID 1596782 の反応式
[CH3:1][O:2][C:3]1[CH:13]=[CH:12][CH:11]=[CH:10][C:4]=1[O:5][CH:6]([CH3:9])[C:7]#[N:8].[H-].[Al+3].[Li+].[H-].[H-].[H-]>C(OCC)C>[CH3:1][O:2][C:3]1[CH:13]=[CH:12][CH:11]=[CH:10][C:4]=1[O:5][CH:6]([CH3:9])[CH2:7][NH2:8]

参加物

4

反応物 2

HCID 21226445Aluminium lithium hydrideHCID 217030942-(2-Methoxy-phenoxy)-propionitrile

生成物 1

HCID 217030831-[(1-Aminopropan-2-YL)oxy]-2-methoxybenzene収率 7%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
65 °C

実験手順

To a solution of 2-(2-methoxy-phenoxy)-propionitrile (3.91 g, 0.022 mol) in anhydrous ethyl ether (30 ml) was added lithium aluminum hydride (1.0 M, 44 ml, 0.044 mol). The mixture was heated at 65° C. for 18 hours and the reaction was quenched with water (3 ml), 15% NaOH (3 ml) and water (9 ml). The resulting material was filtered through celite. The celite was washed with methanol (200 ml), and the solvent was removed under vacuum. Chromatography (10% methanol-methylene chloride) afforded 0.26 g (7%) of product as yellow oil. MS EI m/e 181

後処理

  1. customthe reaction was quenched with water (3 ml), 15% NaOH (3 ml) and water (9 ml)
  2. filtrationThe resulting material was filtered through celite
  3. washThe celite was washed with methanol (200 ml)
  4. customthe solvent was removed under vacuum

出典と根拠

ORDレコード
ord-3a7a633b456e41249f80d843e25042fe
出典データセット
uspto-grants-2001_09
特許番号
US06291683B1

反応ノート

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