Hydrochloric Acid → HCID 135456120, 화합물

HRID 733374노트

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HRID 733374 반응식
[C:1]([C:4]1[CH:5]=[CH:6][C:7]([OH:39])=[C:8]([S:10]([NH:13][CH2:14][CH2:15][C:16]2[CH:21]=[CH:20][C:19]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[S:28]([CH3:31])(=[O:30])=[O:29])=[CH:18][C:17]=2[O:32][CH2:33][C:34]([O:36]CC)=[O:35])(=[O:12])=[O:11])[CH:9]=1)(=[NH:3])[NH2:2].[OH-].[Na+].[ClH:42]>C(#N)C>[ClH:42].[C:1]([C:4]1[CH:5]=[CH:6][C:7]([OH:39])=[C:8]([S:10]([NH:13][CH2:14][CH2:15][C:16]2[CH:21]=[CH:20][C:19]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[S:28]([CH3:31])(=[O:30])=[O:29])=[CH:18][C:17]=2[O:32][CH2:33][C:34]([OH:36])=[O:35])(=[O:11])=[O:12])[CH:9]=1)(=[NH:2])[NH2:3]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 136367330HCID 136367330, 화합물

생성물 1

HCID 135456120HCID 135456120, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of 290 mg of ethyl [4-[2-(5-carbamimidoyl-2-hydroxybenzenesulfonylamino)ethyl]-2′-methanesulfonoyl-biphenyl-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.

후처리

  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

출처 및 근거

ORD 기록
ord-92a5d0342137402e93dc3f63962395bd
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07589126B2

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