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Triethylamine → 1-{2-Oxo-2-[4-(4-pyrimidin-2-yl-phenyl)-piperazin-1-yl]-ethyl}-pyrrolidine-3-carboxylic acid [3-(4-fluoro-phenyl)-1H-indazol-5-yl]-amide

HRID 1037986
ノート
印刷プレビュー

反応式

HRID 1037986 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:16]3[C:11](=[CH:12][CH:13]=[C:14]([NH2:17])[CH:15]=3)[NH:10][N:9]=2)=[CH:4][CH:3]=1.[O:18]=[C:19]([N:29]1[CH2:34][CH2:33][N:32]([C:35]2[CH:40]=[CH:39][C:38]([C:41]3[N:46]=[CH:45][CH:44]=[CH:43][N:42]=3)=[CH:37][CH:36]=2)[CH2:31][CH2:30]1)[CH2:20][N:21]1[CH2:25][CH2:24][CH:23]([C:26](O)=[O:27])[CH2:22]1.C(N(CC)CC)C>CN(C=O)C>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[C:16]3[C:11](=[CH:12][CH:13]=[C:14]([NH:17][C:26]([CH:23]4[CH2:24][CH2:25][N:21]([CH2:20][C:19](=[O:18])[N:29]5[CH2:30][CH2:31][N:32]([C:35]6[CH:40]=[CH:39][C:38]([C:41]7[N:42]=[CH:43][CH:44]=[CH:45][N:46]=7)=[CH:37][CH:36]=6)[CH2:33][CH2:34]5)[CH2:22]4)=[O:27])[CH:15]=3)[NH:10][N:9]=2)=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 224802843-(4-fluorophenyl)-1H-indazol-5-amineHCID 674194121-{2-Oxo-2-[4-(4-pyrimidin-2-yl-phenyl)-piperazin-1-yl]-ethyl}-pyrrolidine-3-carboxylic acid2 回

生成物 1

HCID 674186161-{2-Oxo-2-[4-(4-pyrimidin-2-yl-phenyl)-piperazin-1-yl]-ethyl}-pyrrolidine-3-carboxylic acid [3-(4-fluoro-phenyl)-1H-indazol-5-yl]-amide収率 24.3%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

3-(4-Fluoro-phenyl)-1H-indazol-5-ylamine (0.11 gm, 0.5 mmol) and 1-{2-Oxo-2-[4-(4-pyrimidin-2-yl-phenyl)-piperazin-1-yl]-ethyl}-pyrrolidine-3-carboxylic acid (compound 12 from Step 9, 0.125 gm, 0.25 mmol) were dissolved in 4 ml of DMF. O-(7-azabenzotriazol-1-yl-)-N,N,N,N-tetramethyluronium hexafluorophosphate (HATU) (0.24 gm, 0.63 mmol) and triethylamine (0.1 ml, 0.76 mmol) were added to the reaction mixture and the mixture stirred for 18 hrs. The reaction mixture was added to bring and extracted with dichloromethane. After drying over magnesium sulfate and filtered, the mixture was evaporated and chromatographed to obtain 36.7 mg of title product.

後処理

  1. additionThe reaction mixture was added
  2. extractionextracted with dichloromethane
  3. dry with materialAfter drying over magnesium sulfate
  4. filtrationfiltered
  5. customthe mixture was evaporated
  6. customchromatographed

出典と根拠

ORDレコード
ord-28a69d1d9e274c4eb35d0d6333e45324
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08546404B2

反応ノート

読み込み中…

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