Water → 7-[1-(Pyridin-4-yl)piperidin-4-ylmethoxy]-1,2,3,4-tetrahydroisoquinoline-2-carboxamide oxime dihydrochloride

HRID 412519노트

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HRID 412519 반응식
CS[C:3]([N:5]1[CH2:14][CH2:13][C:12]2[C:7](=[CH:8][C:9]([O:15][CH2:16][CH:17]3[CH2:22][CH2:21][N:20]([C:23]4[CH:28]=[CH:27][N:26]=[CH:25][CH:24]=4)[CH2:19][CH2:18]3)=[CH:10][CH:11]=2)[CH2:6]1)=[NH:4].[ClH:29].[OH:30][NH2:31].C([O-])(=O)C.[Na+].O>C(O)C>[ClH:29].[ClH:29].[N:26]1[CH:27]=[CH:28][C:23]([N:20]2[CH2:21][CH2:22][CH:17]([CH2:16][O:15][C:9]3[CH:8]=[C:7]4[C:12]([CH2:13][CH2:14][N:5]([C:3](=[N:31][OH:30])[NH2:4])[CH2:6]4)=[CH:11][CH:10]=3)[CH2:18][CH2:19]2)=[CH:24][CH:25]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 600641917-[1-(Pyridin-4-yl)piperidin-4-ylmethoxy]-1,2,3,4-tetrahydroisoquinoline-2-carbothioimidic acid methyl ester

생성물 1

HCID 865907237-[1-(Pyridin-4-yl)piperidin-4-ylmethoxy]-1,2,3,4-tetrahydroisoquinoline-2-carboxamide oxime dihydrochloride수율 53.4%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
40 °C

실험 절차

To a solution of 7-[1-(pyridin-4-yl)piperidin-4-ylmethoxy]-1,2,3,4-tetrahydroisoquinoline-2-carbothioimidic acid methyl ester (135 mg) in ethanol (3 ml) were added hydroxyamine hydrochloride (47 mg) and sodium acetate (56 mg), and the mixture was stirred at 40° C. for 2 hours. After completion of the reaction, water was added and the mixture was washed with chloroform. Thereto was added 4N aqueous sodium hydroxide solution, and the mixture was extracted with chloroform. The organic layer was washed successively with water and saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated and the obtained solid was treated with hydrogen chloride—ethanol solution and dried under reduced pressure to give the title compound (82 mg).

후처리

  1. additionwas added
  2. washthe mixture was washed with chloroform
  3. additionThereto was added 4N aqueous sodium hydroxide solution
  4. extractionthe mixture was extracted with chloroform
  5. washThe organic layer was washed successively with water and saturated brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe solvent was evaporated
  8. additionthe obtained solid was treated with hydrogen chloride—ethanol solution
  9. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-3717f1f56fb646758527645694fa2841
출처 데이터셋
uspto-grants-2003_05
특허 번호
US06562828B1

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