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

HRID 1954235ノート

反応式

HRID 1954235 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 (M+).

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-38d91e679b8144c29a7846946780722e
出典データセット
uspto-grants-2000_09
特許番号
US06121307

反応ノート

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