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Trifluoroacetic acid → HCID 22708205、化合物

HRID 1266532
ノート
印刷プレビュー

反応式

HRID 1266532 の反応式
[CH3:1][O:2][CH2:3][CH2:4][N:5]([CH2:23][C:24]1[CH:40]=[CH:39][C:27]([O:28][C:29]([CH3:38])([CH3:37])[C:30]([O:32]C(C)(C)C)=[O:31])=[CH:26][CH:25]=1)[CH2:6][C:7]([NH:9][C:10]1[CH:15]=[CH:14][C:13]([CH:16]([CH3:18])[CH3:17])=[CH:12][C:11]=1[C:19]([F:22])([F:21])[F:20])=[O:8].FC(F)(F)C(O)=O>ClCCl>[CH3:1][O:2][CH2:3][CH2:4][N:5]([CH2:23][C:24]1[CH:25]=[CH:26][C:27]([O:28][C:29]([CH3:38])([CH3:37])[C:30]([OH:32])=[O:31])=[CH:39][CH:40]=1)[CH2:6][C:7]([NH:9][C:10]1[CH:15]=[CH:14][C:13]([CH:16]([CH3:18])[CH3:17])=[CH:12][C:11]=1[C:19]([F:22])([F:21])[F:20])=[O:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 22708262HCID 22708262、化合物

生成物 1

HCID 22708205HCID 22708205、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

0.842 g (1.49 mmol) of the compound from Example 3-7 is initially charged in 10 ml of dichloromethane. At room temperature, 10 ml of trifluoroacetic acid are added. The reaction mixture is stirred at room temperature for 2 hours. The mixture is then concentrated under reduced pressure using a rotary evaporator. The residue is taken up in ethyl acetate and washed with water, 20% strength sodium acetate solution, water and saturated sodium chloride solution. The organic phase is dried over magnesium sulphate and freed from the solvent under reduced pressure. The product is purified chromatographically on silica gel (dichloromethane/methanol 30:1) and then dried under reduced pressure. This gives 0.648 g (85% of theory) of the title compound.

後処理

  1. concentrationThe mixture is then concentrated under reduced pressure
  2. customa rotary evaporator
  3. washwashed with water, 20% strength sodium acetate solution, water and saturated sodium chloride solution
  4. dry with materialThe organic phase is dried over magnesium sulphate
  5. customThe product is purified chromatographically on silica gel (dichloromethane/methanol 30:1)
  6. customdried under reduced pressure

出典と根拠

ORDレコード
ord-988380cd7ee8422da7d0eaa609dbb0f8
出典データセット
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06548538B2

反応ノート

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