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Lithium hydroxide, monohydrate → [(Z)-1-[4-(2-Biphenylylcarbonylamino)benzoyl]-4,4-difluoro-2,3,4,5-tetrahydro-1H-1-benzazepine-5-ylidene]acetic acid

HRID 726708
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HRID 726708 반응식
[F:1][C:2]1([F:41])[CH2:3][CH2:4][N:5]([C:18](=[O:40])[C:19]2[CH:24]=[CH:23][C:22]([NH:25][C:26](=[O:39])[C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=3[C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)=[CH:21][CH:20]=2)[C:6]2[CH:17]=[CH:16][CH:15]=[CH:14][C:7]=2/[C:8]/1=[CH:9]/[C:10]([O:12]C)=[O:11].O.[OH-].[Li+]>CO>[F:41][C:2]1([F:1])[CH2:3][CH2:4][N:5]([C:18](=[O:40])[C:19]2[CH:24]=[CH:23][C:22]([NH:25][C:26](=[O:39])[C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=3[C:33]3[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=3)=[CH:21][CH:20]=2)[C:6]2[CH:17]=[CH:16][CH:15]=[CH:14][C:7]=2/[C:8]/1=[CH:9]/[C:10]([OH:12])=[O:11]
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참가 물질

4

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 10602784[(Z)-1-[4-(2-Biphenylylcarbonylamino)benzoyl]-4,4-difluoro-2,3,4,5-tetrahydro-1H-1-benzazepine-5-ylidene]acetic acid methyl ester

생성물 1

HCID 10554393[(Z)-1-[4-(2-Biphenylylcarbonylamino)benzoyl]-4,4-difluoro-2,3,4,5-tetrahydro-1H-1-benzazepine-5-ylidene]acetic acid수율 75.8%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Methyl (Z)-[4,4-difluoro-1-[4-(2phenylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-1-benzazepin-5-ylidene]acetate (857 mg) was dissolved in 10 ml of methanol, 2 ml of aqueous solution containing 195 mg of lithium hydroxide monohydrate was added dropwise to the above solution under ice-cooling, and the mixture was stirred at room temperature for 7 hours. After evaporating the solvent under a reduced pressure, 1N hydrochloric acid aqueous solution was added, and the mixture was extracted with chloroform and dried over anhydrous magnesium sulfate. After evaporation of the solvent under a reduced pressure, the resulting residue was recrystallized from ethyl acetatehexane to obtain 633 mg of (Z)-[4,4-difluoro-1-[4-(2-phenylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-1-benzazepin-5-ylidene]acetic acid.

후처리

  1. additionwas added dropwise to the above solution under ice-
  2. temperaturecooling
  3. customAfter evaporating the solvent under a reduced pressure, 1N hydrochloric acid aqueous solution
  4. additionwas added
  5. extractionthe mixture was extracted with chloroform
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customAfter evaporation of the solvent under a reduced pressure
  8. customthe resulting residue was recrystallized from ethyl acetatehexane

출처 및 근거

ORD 기록
ord-0ac6d333e3e14c50b4391bf4f72bbef0
출처 데이터셋
uspto-grants-1998_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05710150

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