Ethyl chloroformate → HCID 131728153、化合物

HRID 13362

反応式

HRID 13362 の反応式
Cl[C:2]([O:4][CH2:5][CH3:6])=[O:3].[NH2:7][C:8]1[N:13]=[CH:12][C:11]([O:14][C:15]2[C:16]([CH:30]3[CH2:34][CH2:33][CH2:32][N:31]3[C:35](=[O:37])[CH3:36])=[CH:17][C:18]3[NH:22][C:21]([C:23]4[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=4)=[N:20][C:19]=3[CH:29]=2)=[CH:10][CH:9]=1>N1C=CC=CC=1>[CH2:5]([O:4][C:2](=[O:3])[NH:7][C:8]1[CH:9]=[CH:10][C:11]([O:14][C:15]2[C:16]([CH:30]3[CH2:34][CH2:33][CH2:32][N:31]3[C:35](=[O:37])[CH3:36])=[CH:17][C:18]3[NH:22][C:21]([C:23]4[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=4)=[N:20][C:19]=3[CH:29]=2)=[CH:12][N:13]=1)[CH3:6]

参加物

4

反応物 2

HCID 10928Ethyl chloroformateHCID 231453671-(2-(6-(6-amino-pyridin-3-yloxy)-2-pyridin-2-yl-3H-benzimidazol-5-yl)-pyrrolidin-1-yl)-ethanone

生成物 1

HCID 131728153HCID 131728153、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

0.003 ml of ethyl chloroformate was added to a pyridine (1 ml) solution of 14.4 mg of 1-(2-(6-(6-amino-pyridin-3-yloxy)-2-pyridin-2-yl-3H-benzimidazol-5-yl)-pyrrolidin-1-yl)-ethanone obtained in Example 340 (step 1), and the reaction liquid was stirred at room temperature for 30 minutes. The reaction liquid was distilled under reduced pressure, and the resulting residue was dissolved in 1 ml of trifluoroacetic acid, and the reaction liquid was stirred at room temperature for 1 hour. The reaction liquid was distilled under reduced pressure, and the resulting residue was purified through reversed-phase middle-pressure liquid chromatography [ODS-AS-360-CC (by YMC), mobile phase: water-acetonitrile-0.1% trifluoroacetic acid] and through silica gel column chromatography (developing solvent: chloroform/methanol=9/1) to obtain the entitled compound as a yellow oily substance.

後処理

  1. customthe reaction liquid
  2. customThe reaction liquid
  3. distillationwas distilled under reduced pressure
  4. dissolutionthe resulting residue was dissolved in 1 ml of trifluoroacetic acid
  5. customthe reaction liquid
  6. stirringwas stirred at room temperature for 1 hour
  7. customThe reaction liquid
  8. distillationwas distilled under reduced pressure
  9. customthe resulting residue was purified through reversed-phase middle-pressure liquid chromatography [ODS-AS-360-CC (by YMC), mobile phase: water-acetonitrile-0.1% trifluoroacetic acid] and through silica gel column chromatography (developing solvent: chloroform/methanol=9/1)
  10. customto obtain the entitled compound as a yellow oily substance

出典と根拠

ORDレコード
ord-2a0180ebe4b145b8a883237ce4e9197a
出典データセット
uspto-grants-2010_06
特許番号
US07728025B2

関連ノート

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