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N,N-Diethyl-1,3-propanediamine → N-[3-(diethylamino)propyl]-4-(4-methoxyphenyl)-5-phenyl-1H-pyrazole-1-acetamide

HRID 704831
ノート
印刷プレビュー

反応式

HRID 704831 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:10]=[N:11][N:12]([CH2:20][C:21]([O:23]CC)=O)[C:13]=2[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[CH:5][CH:4]=1.[CH2:26]([N:28]([CH2:31][CH2:32][CH2:33][NH2:34])[CH2:29][CH3:30])[CH3:27]>>[CH2:26]([N:28]([CH2:29][CH3:30])[CH2:31][CH2:32][CH2:33][NH:34][C:21](=[O:23])[CH2:20][N:12]1[C:13]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[C:9]([C:6]2[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)[CH:10]=[N:11]1)[CH3:27]
参加物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 61011N,N-Diethyl-1,3-propanediamineHCID 14699555Ethyl 4-(4-methoxyphenyl)-5-phenyl-1H-pyrazole-1-acetate

生成物 1

HCID 14699593N-[3-(diethylamino)propyl]-4-(4-methoxyphenyl)-5-phenyl-1H-pyrazole-1-acetamide

実験手順

A solution of 7.5 g (0.022 mol) of ethyl 4-(4-methoxyphenyl)-5-phenyl-1H-pyrazole-1-acetate of example 4 in 35 mL of diethylaminopropylamine was stirred on a steam bath under nitrogen for 14 hours. The diethylaminopropylamine was removed in vacuo and the residue taken up in 200 mL of ethyl acetate. The ethyl acetate solution was washed twice with water, once with brine, and dried over sodium sulfate. The solvent was removed in vacuo and the residue was distilled in a Kugelrohr at 250° C./0.1 mm to yield 6.39 g of N-[3-(diethylamino)propyl]-4-(4-methoxyphenyl)-5-phenyl-1H-pyrazole-1-acetamide as a clear viscous amber oil.

後処理

  • customThe diethylaminopropylamine was removed in vacuo
  • washThe ethyl acetate solution was washed twice with water, once with brine
  • dry with materialdried over sodium sulfate
  • customThe solvent was removed in vacuo
  • distillationthe residue was distilled in a Kugelrohr at 250° C./0.1 mm
  • 出典と根拠

    ORDレコード
    ord-92ff39f1a4d745a4a219c3d7e8d06a50
    出典データセット
    uspto-grants-1991_01
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US04988725

    反応ノート

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