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Trifluoroacetic acid → 3-(5-methyl-4-phenyl-1H-imidazol-2-yl)-3,4-dihydro-1H-isoquinoline

HRID 1270818
ノート
印刷プレビュー

反応式

HRID 1270818 の反応式
C(O)(C(F)(F)F)=O.C(OC([N:15]1[CH:24]([C:25]2[NH:26][C:27]([CH3:36])=[C:28]([C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=3)[N:29]=2)[CH2:23][C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH2:16]1)=O)(C)(C)C>>[CH3:36][C:27]1[NH:26][C:25]([CH:24]2[CH2:23][C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[CH2:16][NH:15]2)=[N:29][C:28]=1[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1
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 6422Trifluoroacetic acidHCID 23570722HCID 23570722、化合物

生成物 1

HCID 219141423-(5-methyl-4-phenyl-1H-imidazol-2-yl)-3,4-dihydro-1H-isoquinoline

実験手順

To a solution of TFA (5 mL) cooled to about 0° C. was added the compound prepared in Step A above (1.10 g, 2.82 mmol), and the reaction mixture stirred for about 30 minutes. The reaction mixture was then removed from the ice bath and allowed to warm to room temperature. Excess TFA was removed under a stream of N2. The residue was partitioned between saturated NaHCO3 and dichloromethane. The aqueous phase was washed with a second portion of dichloromethane and the organic phases combined. The combined organic phase was dried over Na2SO4, then filtered to yield the title product as a solution in dichloromethane, which was used without further purification or isolation.

後処理

  1. customThe reaction mixture was then removed from the ice bath
  2. custom
Excess TFA was removed under a stream of N2
  • customThe residue was partitioned between saturated NaHCO3 and dichloromethane
  • washThe aqueous phase was washed with a second portion of dichloromethane
  • dry with materialThe combined organic phase was dried over Na2SO4
  • filtrationfiltered
  • 出典と根拠

    ORDレコード
    ord-15f1383959394cefa5c45177b28985ff
    出典データセット
    uspto-grants-2007_04
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US07202381B2

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