4-(3-{4-[(4-Chloro-phenyl)-methyl-carbamoyl]-2-fluoro-phenoxy}-propyl)-piperazine-1-carboxylic Acid Tert-butyl Ester → N-(4-Chloro-phenyl)-3-fluoro-N-methyl-4-(3-piperazin-1-yl-propoxy)-benzamide Dihydrochloride

HRID 220908ノート

反応式

HRID 220908 の反応式
C(OC([N:8]1[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][O:17][C:18]2[CH:23]=[CH:22][C:21]([C:24](=[O:34])[N:25]([C:27]3[CH:32]=[CH:31][C:30]([Cl:33])=[CH:29][CH:28]=3)[CH3:26])=[CH:20][C:19]=2[F:35])[CH2:10][CH2:9]1)=O)(C)(C)C>Cl.O1CCOCC1>[ClH:33].[ClH:33].[Cl:33][C:30]1[CH:31]=[CH:32][C:27]([N:25]([CH3:26])[C:24](=[O:34])[C:21]2[CH:22]=[CH:23][C:18]([O:17][CH2:16][CH2:15][CH2:14][N:11]3[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]3)=[C:19]([F:35])[CH:20]=2)=[CH:28][CH:29]=1

参加物

4

反応物 1

HCID 575552734-(3-{4-[(4-Chloro-phenyl)-methyl-carbamoyl]-2-fluoro-phenoxy}-propyl)-piperazine-1-carboxylic Acid Tert-butyl Ester

生成物 1

HCID 67287537N-(4-Chloro-phenyl)-3-fluoro-N-methyl-4-(3-piperazin-1-yl-propoxy)-benzamide Dihydrochloride収率 100%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 312751,4-Dioxane溶媒

実験手順

4-(3-{4-[(4-Chloro-phenyl)-methyl-carbamoyl]-2-fluoro-phenoxy}-propyl)-piperazine-1-carboxylic acid tert-butyl ester from Example E71.1 (210 mg, 0.4 mmol) was dissolved in 4M HCl in dioxan (5 ml) and stirred for 1 h at room temperature. Solvents were concentrated in vacuo and azeotroped with toluene to yield the title compound (184 mg, 100%).

後処理

  1. concentrationSolvents were concentrated in vacuo
  2. customazeotroped with toluene

出典と根拠

ORDレコード
ord-208686396b43479a84f22d4758bcb970
出典データセット
uspto-grants-2012_06
特許番号
US08202858B2

反応ノート

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