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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 1010327
ノート
印刷プレビュー

反応式

HRID 1010327 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 mixture was concentrated under reduced pressure, saturated sodium bicarnobate 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 brine, 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 mixture was concentrated under reduced pressure, saturated sodium bicarnobate water
  2. additionwas added to alkalinity
  3. customliquid separation and extraction
  4. washThe organic layer was washed with saturated brine
  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-c72f9b7ab731434084e51c63eb0c83e1
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07973160B2

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