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Trifluoroacetic acid → 1-{2-Chloro-4-[6-(4-hydroxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-4-yloxy]-phenyl}-3-cyclopropylurea

HRID 387934
ノート
印刷プレビュー

反応式

HRID 387934 の反応式
FC(F)(F)C(O)=O.C1(SC)C=CC=CC=1.C([O:23][C:24]1[CH:29]=[CH:28][C:27]([C:30]2[NH:53][C:33]3[N:34]=[CH:35][N:36]=[C:37]([O:38][C:39]4[CH:44]=[CH:43][C:42]([NH:45][C:46]([NH:48][CH:49]5[CH2:51][CH2:50]5)=[O:47])=[C:41]([Cl:52])[CH:40]=4)[C:32]=3[CH:31]=2)=[CH:26][CH:25]=1)C1C=CC=CC=1>>[Cl:52][C:41]1[CH:40]=[C:39]([O:38][C:37]2[C:32]3[CH:31]=[C:30]([C:27]4[CH:26]=[CH:25][C:24]([OH:23])=[CH:29][CH:28]=4)[NH:53][C:33]=3[N:34]=[CH:35][N:36]=2)[CH:44]=[CH:43][C:42]=1[NH:45][C:46]([NH:48][CH:49]1[CH2:50][CH2:51]1)=[O:47]
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

4

反応物 3

HCID 6422Trifluoroacetic acidHCID 7520ThioanisoleHCID 589310291-{4-[6-(4-Benzyloxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-4-yloxy]-2-chlorophenyl}-3-cyclopropylurea

生成物 1

HCID 589313921-{2-Chloro-4-[6-(4-hydroxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-4-yloxy]-phenyl}-3-cyclopropylurea収率 75.4%

反応条件

温度
45 °C

実験手順

After adding 2 ml of trifluoroacetic acid and 0.1 ml of thioanisole to 24 mg of 1-{4-[6-(4-benzyloxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-4-yloxy]-2-chlorophenyl}-3-cyclopropylurea, the mixture was stirred at 45° C. for 30 minutes. The reaction system was concentrated under reduced pressure, saturated bicarbonate water was added to alkalinity, and then liquid separation and extraction were performed with ethyl acetate and tetrahydrofuran. The organic layer was washed with saturated saline, dried over anhydrous sodium sulfate, concentrated and dried under reduced pressure to obtain 15 mg of the title compound.

後処理

  1. concentrationThe reaction system was concentrated under reduced pressure, saturated bicarbonate water
  2. additionwas added to alkalinity
  3. customliquid separation and extraction
  4. washThe organic layer was washed with saturated saline
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated
  7. customdried under reduced pressure

出典と根拠

ORDレコード
ord-5ecbf81abdee42f4821873a1e0a0c822
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08372981B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート