Water → HCID 54146616, 화합물

HRID 344445노트

반응식

HRID 344445 반응식
C(=O)([O-])[O-].[K+].[K+].Br[CH2:8][CH2:9][CH2:10][CH2:11][C:12]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)=[O:13].Cl.Cl.[NH2:22][C:23]1[C:38]([Cl:39])=[CH:37][C:26]([C:27]([NH:29][CH2:30][CH:31]2[CH2:36][CH2:35][NH:34][CH2:33][CH2:32]2)=[O:28])=[C:25]([O:40][CH3:41])[CH:24]=1.O>CN(C)C=O>[NH2:22][C:23]1[C:38]([Cl:39])=[CH:37][C:26]([C:27]([NH:29][CH2:30][CH:31]2[CH2:32][CH2:33][N:34]([CH2:8][CH2:9][CH2:10][CH2:11][C:12](=[O:13])[C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[CH2:35][CH2:36]2)=[O:28])=[C:25]([O:40][CH3:41])[CH:24]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 111840715-bromo-1-phenyl-1-pentanoneHCID 699663304-amino-5-chloro-2-methoxy-N-(piperidin-4-ylmethyl)benzamide dihydrochloride

생성물 1

HCID 54146616HCID 54146616, 화합물수율 52.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Potassium carbonate (0.57 g) and 5-bromo-1-phenyl-1-pentanone (0.80 g) were added to a solution (45 ml) of 4-amino-5-chloro-2-methoxy-N-(piperidin-4-ylmethyl)benzamide dihydrochloride (1.5 g) in dimethylformamide, and the mixture was stirred at 70°-80° C. for 7.5 hr. Water was added to the reaction mixture, and the mixture was extracted with chloroform. The organic layer was washed with saturated aqueous sodium chloride solution, dried and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to give crystals. The obtained crystals were recrystallized from ethyl acetate to give 0.80 g of 4-amino-5-chloro-2-methoxy-N-((1-(5-oxo-5-phenylpentyl)piperidin-4-yl)methyl)benzamide.

후처리

  1. extractionthe mixture was extracted with chloroform
  2. washThe organic layer was washed with saturated aqueous sodium chloride solution
  3. customdried
  4. customthe solvent was evaporated under reduced pressure
  5. customThe obtained residue was purified by silica gel column chromatography
  6. customto give crystals
  7. customThe obtained crystals were recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-6191d1722cc94edb9774336c2cf38d46
출처 데이터셋
uspto-grants-1999_01
특허 번호
US05864039

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