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Ammonium Chloride → 4-Methyl-1-phenylpent-1-yn-3-amine

HRID 1711989
ノート
印刷プレビュー

反応式

HRID 1711989 の反応式
[CH3:1][CH:2]([CH3:19])[CH:3]([N:12]1CCC(=O)CC1)[C:4]#[C:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[Cl-].[NH4+]>>[CH3:1][CH:2]([CH3:19])[CH:3]([NH2:12])[C:4]#[C:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 25517Ammonium ChlorideHCID 68500493HCID 68500493、化合物

生成物 1

HCID 125232624-Methyl-1-phenylpent-1-yn-3-amine収率 64.1%

反応条件

温度
90 °C

実験手順

A 25 ml pressure tube was charged with 1-(4-methyl-1-phenylpent-1-yn-3-yl)piperidin-4-one (76.6 mg, 0.30 mmol) and ammonium chloride (48 mg, 0.90 mmol). The pressure tube was purged with argon for 5 min and then saturated ethanolic ammonia solution (2 ml) was added. The pressure tube was sealed tightly and the reaction mixture was stirred at 90° C. for 4 hrs. The reaction mixture was concentrated under reduced pressure and the brown residue was subjected to flash chromatography on silica gel (EtOAc/MeOH=19:1) to give 33.3 mg of a pure title compound as a yellowish oil. (yield: 64%)

後処理

  • customThe pressure tube was purged with argon for 5 min
  • additionsaturated ethanolic ammonia solution (2 ml) was added
  • customThe pressure tube was sealed tightly
  • concentrationThe reaction mixture was concentrated under reduced pressure
  • 出典と根拠

    ORDレコード
    ord-f91ebca499ba4e3e976ee331babdcd82
    出典データセット
    uspto-grants-2010_09
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US07790882B2

    反応ノート

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