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

HRID 1954235노트

반응식

HRID 1954235 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
65 °C

실험 절차

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+).

후처리

  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

출처 및 근거

ORD 기록
ord-38d91e679b8144c29a7846946780722e
출처 데이터셋
uspto-grants-2000_09
특허 번호
US06121307

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