Ethyl chloroformate → ethyl 2-(5-(4-fluorophenoxy)-2-(pyridin-2-yl)-1H-benzo[d]imidazol-6-yl)pyrrolidine-1-carboxylate

HRID 13283

反応式

HRID 13283 の反応式
Cl[C:2]([O:4][CH2:5][CH3:6])=[O:3].[F:7][C:8]1[CH:34]=[CH:33][C:11]([O:12][C:13]2[C:27]([CH:28]3[CH2:32][CH2:31][CH2:30][NH:29]3)=[CH:26][C:16]3[NH:17][C:18]([C:20]4[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=4)=[N:19][C:15]=3[CH:14]=2)=[CH:10][CH:9]=1>[Zn].C1C=CC=CC=1>[F:7][C:8]1[CH:9]=[CH:10][C:11]([O:12][C:13]2[C:27]([CH:28]3[CH2:32][CH2:31][CH2:30][N:29]3[C:2]([O:4][CH2:5][CH3:6])=[O:3])=[CH:26][C:16]3[NH:17][C:18]([C:20]4[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=4)=[N:19][C:15]=3[CH:14]=2)=[CH:33][CH:34]=1

参加物

5

反応物 2

HCID 10928Ethyl chloroformateHCID 231455755-(4-fluoro-phenoxy)-2-pyridin-2-yl-6-pyrrolidin-2-yl-1H-benzimidazole

生成物 1

HCID 23145223ethyl 2-(5-(4-fluorophenoxy)-2-(pyridin-2-yl)-1H-benzo[d]imidazol-6-yl)pyrrolidine-1-carboxylate

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 241Benzene溶媒

実験手順

5.2 mg of zinc powder and 0.006 ml of ethyl chloroformate were added in order to a benzene (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.

後処理

  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)

出典と根拠

ORDレコード
ord-3e5e65171b8849119f3790876982c93e
出典データセット
uspto-grants-2010_06
特許番号
US07728025B2

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