Ethyl chloroformate → HCID 131728153, 화합물

HRID 13362

반응식

HRID 13362 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 131728153HCID 131728153, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2a0180ebe4b145b8a883237ce4e9197a
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728025B2

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