Hydrochloric Acid → HCID 135456120、化合物

HRID 229604ノート

反応式

HRID 229604 の反応式
C([O:3][C:4](=[O:39])[CH2:5][O:6][C:7]1[CH:8]=[C:9]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=2[S:35]([CH3:38])(=[O:37])=[O:36])[CH:10]=[CH:11][C:12]=1[CH2:13][CH2:14][NH:15][S:16]([C:19]1[CH:24]=[C:23]([C:25](=[NH:27])[NH2:26])[CH:22]=[CH:21][C:20]=1[OH:28])(=[O:18])=[O:17])C.[OH-].[Na+].[ClH:42]>C(#N)C>[ClH:42].[C:25]([C:23]1[CH:22]=[CH:21][C:20]([OH:28])=[C:19]([S:16]([NH:15][CH2:14][CH2:13][C:12]2[CH:11]=[CH:10][C:9]([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=3[S:35]([CH3:38])(=[O:37])=[O:36])=[CH:8][C:7]=2[O:6][CH2:5][C:4]([OH:39])=[O:3])(=[O:17])=[O:18])[CH:24]=1)(=[NH:26])[NH2:27]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 136367330HCID 136367330、化合物

生成物 1

HCID 135456120HCID 135456120、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a solution of 290 mg of ethyl[4-[2-(5-carbamimidoyl-2-hydroxybenzenesulfonylamino)ethyl]-2′-methanesulfonoylbiphenyl-3-yloxy]acetate in 1.0 mL of acetonitrile was added 0.756 mL of 2 mol/L sodium hydroxide solution, and the mixture was stirred at room temperature for 30 minutes. To the reaction mixture was added 1.26 mL of 2 mol/L hydrochloric acid, and the mixture was concentrated under reduced pressure. To the residue was added water, and the mixture was purified by column chromatography on trimethylaminopropylated silica gel (eluent: 10% 1 mol/L hydrochloric acid-acetonitrile). The eluent was concentrated under reduced pressure to give 260 mg of [4-[2-(5-carbamimidoyl-2-hydroxybenzenesulfonylamino)-ethyl]-2′-methanesulfonoylbiphenyl-3-yloxy]acetic acid hydrochloride as a white solid.

後処理

  1. concentrationthe mixture was concentrated under reduced pressure
  2. additionTo the residue was added water
  3. customthe mixture was purified by column chromatography on trimethylaminopropylated silica gel (eluent: 10% 1 mol/L hydrochloric acid-acetonitrile)
  4. concentrationThe eluent was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-30d5797912c04e949378954cdcd36fe9
出典データセット
uspto-grants-2009_07
特許番号
US07563822B2

反応ノート

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