Triethylamine → 5-(4-Fluoro-phenoxy)-6-(1-methanesulfonyl-pyrrolidin-2-yl)-2-pyridin-2-yl-1H-benzimidazole

HRID 13280

반응식

HRID 13280 반응식
C(N(CC)CC)C.[CH3:8][S:9](Cl)(=[O:11])=[O:10].[F:13][C:14]1[CH:40]=[CH:39][C:17]([O:18][C:19]2[C:33]([CH:34]3[CH2:38][CH2:37][CH2:36][NH:35]3)=[CH:32][C:22]3[NH:23][C:24]([C:26]4[CH:31]=[CH:30][CH:29]=[CH:28][N:27]=4)=[N:25][C:21]=3[CH:20]=2)=[CH:16][CH:15]=1>C(OCC)(=O)C>[F:13][C:14]1[CH:15]=[CH:16][C:17]([O:18][C:19]2[C:33]([CH:34]3[CH2:38][CH2:37][CH2:36][N:35]3[S:9]([CH3:8])(=[O:11])=[O:10])=[CH:32][C:22]3[NH:23][C:24]([C:26]4[CH:31]=[CH:30][CH:29]=[CH:28][N:27]=4)=[N:25][C:21]=3[CH:20]=2)=[CH:39][CH:40]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 231455755-(4-fluoro-phenoxy)-2-pyridin-2-yl-6-pyrrolidin-2-yl-1H-benzimidazole

생성물 1

HCID 231455565-(4-Fluoro-phenoxy)-6-(1-methanesulfonyl-pyrrolidin-2-yl)-2-pyridin-2-yl-1H-benzimidazole

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

0.01 ml of triethylamine and 0.005 ml of methanesulfonyl chloride were added in order to an ethyl acetate (1 ml) solution of 20 mg of 5-(4-fluoro-phenoxy)-2-pyridin-2-yl-6-pyrrolidin-2-yl-1H-benzimidazole obtained in Example 168, and the reaction liquid was stirred overnight at room temperature. The reaction solvent was evaporated away under reduced pressure, and the resulting residue was purified through partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=10/1) to obtain the entitled compound as a white solid.

후처리

  1. customthe reaction liquid
  2. customThe reaction solvent was evaporated away under reduced pressure
  3. customthe resulting residue was purified
  4. customthrough partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=10/1)

출처 및 근거

ORD 기록
ord-723885e8e8d842f0956be8a09d9fef6e
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728025B2

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