Sodium Carbonate → HCID 15087792, 화합물

HRID 1073165노트

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HRID 1073165 반응식
Cl[CH2:2][CH2:3][CH2:4][CH2:5][N:6]([C:15]1[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=1)[C:7]([C:9]1[CH:10]=[N:11][CH:12]=[CH:13][CH:14]=1)=[O:8].[CH3:22][CH:23]1[CH2:28][NH:27][CH2:26][CH2:25][N:24]1[C:29]([O:31][C:32]([CH3:35])([CH3:34])[CH3:33])=[O:30].C(=O)([O-])[O-].[Na+].[Na+]>CN(C)C=O>[F:21][C:18]1[CH:19]=[CH:20][C:15]([N:6]([C:7]([C:9]2[CH:10]=[N:11][CH:12]=[CH:13][CH:14]=2)=[O:8])[CH2:5][CH2:4][CH2:3][CH2:2][N:27]2[CH2:26][CH2:25][N:24]([C:29]([O:31][C:32]([CH3:35])([CH3:34])[CH3:33])=[O:30])[CH:23]([CH3:22])[CH2:28]2)=[CH:16][CH:17]=1

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 15087784tert-Butyl 2-methylpiperazine-1-carboxylateHCID 15087790N-(4-Chlorobutyl)-N-(4-fluorophenyl)-3-pyridinecarboxamide

생성물 1

HCID 15087792HCID 15087792, 화합물수율 57.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
90 °C

실험 절차

A mixture of 5 parts of N-(4-chlorobutyl)-N-(4-fluorophenyl)-3-pyridinecarboxamide, 2.77 parts of (1,1-dimethylethyl) 2-methyl-1-piperazinecarboxylate, 1.58 parts of sodium carbonate and 94 parts of N,N-dimethylformamide was stirred for 48 hours at 90° C. The reaction mixture was evaporated and the residue was taken up in water. The product was extracted twice with dichloromethane. The combined extracts were washed with water, dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (96:4 by volume) as eluent. The first fraction was collected and the eluent was evaporated, yielding 3.5 parts (57.2%) of (1,1-dimethylethyl) 4-[4-[(4-fluorophenyl)(3-pyridinylcarbonyl)amino]butyl]-2-methyl-1-piperazinecarboxylate as a residue (int. 43).

후처리

  1. customThe reaction mixture was evaporated
  2. extractionThe product was extracted twice with dichloromethane
  3. washThe combined extracts were washed with water
  4. customdried
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue was purified by column chromatography over silica gel using
  8. additiona mixture of trichloromethane and methanol (96:4 by volume) as eluent
  9. customThe first fraction was collected
  10. customthe eluent was evaporated

출처 및 근거

ORD 기록
ord-6c4ee06b84424d6e9a31040b37824cea
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04968684

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