Trifluoroacetic acid → HCID 21100737、化合物

HRID 1352513ノート

反応式

HRID 1352513 の反応式
FC(F)(F)C(O)=O.C(OC(=O)[NH:14][C:15]1[CH:20]=[CH:19][C:18]([C:21]2[C:25]([CH2:26][C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)=[CH:24][O:23][N:22]=2)=[CH:17][CH:16]=1)(C)(C)C>>[CH2:26]([C:25]1[C:21]([C:18]2[CH:17]=[CH:16][C:15]([NH2:14])=[CH:20][CH:19]=2)=[N:22][O:23][CH:24]=1)[C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1

参加物

3

反応物 2

HCID 6422Trifluoroacetic acidHCID 69422093HCID 69422093、化合物

生成物 1

HCID 21100737HCID 21100737、化合物収率 70%

実験手順

Trifluoroacetic acid (0.5 mL) is added to [4-(4-benzylisoxazol-3-yl)phenyl]carbamic acid tert-butyl ester (0.3 g) and stirred for 30 minutes. The reaction mixture is concentrated under reduced pressure and the concentrate is partitioned between ethyl acetate and 1N sodium hydroxide solution. The organic layer is washed with saturated sodium chloride, dried over anhydrous magnesium sulfate and chromatographed on silica gel (ethyl acetate/hexane as eluant) to give 0.15 g product as a white solid. MS: m/z 251 (M+H)+.

後処理

  1. concentrationThe reaction mixture is concentrated under reduced pressure
  2. customthe concentrate is partitioned between ethyl acetate and 1N sodium hydroxide solution
  3. washThe organic layer is washed with saturated sodium chloride
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customchromatographed on silica gel (ethyl acetate/hexane as eluant)

出典と根拠

ORDレコード
ord-c517227dcce74e24ba87c98372128d96
出典データセット
uspto-grants-2007_05
特許番号
US07220768B2

反応ノート

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