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Hydrochloric Acid → 2-Methyl-4-(piperidin-1-yl)-N-(3-(trifluoromethyl)benzyl)-1,8-naphthyridine-3-carboxamide

HRID 1961466
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HRID 1961466 반응식
[CH3:1][C:2]1[C:11]([C:12]([O:14]CC)=O)=[C:10]([N:17]2[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]2)[C:9]2[C:4](=[N:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[OH-].[Na+].Cl.Cl.CN(C)CCCN=C=NCC.O.ON1C2C=CC=CC=2N=N1.CCN(CC)CC.[F:56][C:57]([F:67])([F:66])[C:58]1[CH:59]=[C:60]([CH:63]=[CH:64][CH:65]=1)[CH2:61][NH2:62]>CCO.O>[CH3:1][C:2]1[C:11]([C:12]([NH:62][CH2:61][C:60]2[CH:63]=[CH:64][CH:65]=[C:58]([C:57]([F:56])([F:66])[F:67])[CH:59]=2)=[O:14])=[C:10]([N:17]2[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22]2)[C:9]2[C:4](=[N:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1
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참가 물질

10

반응물 7

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 759623-(Trifluoromethyl)benzylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 66634229HCID 66634229, 화합물

생성물 1

HCID 469085792-Methyl-4-(piperidin-1-yl)-N-(3-(trifluoromethyl)benzyl)-1,8-naphthyridine-3-carboxamide수율 12%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

Ethyl 2-methyl-4-(piperidin-1-yl)-1,8-naphthyridine-3-carboxylate (120.0 mg, 0.4 mmol) was dissolved in EtOH. NaOH (4.0 ml of a 1.0 M aq. solution) was added and the mixture refluxed for 3.0 days. The mixture was cooled, acidified with aq. HCl (1.0 M) and concentrated to dryness. The residue was suspended in anhydrous THF, N-(3-dimethylaminopropyl)-N′-ethyl-carbodiimide hydrochloride (84.34 mg, 0.44 mmol), 1-hydroxybenzotriazole hydrate (30.74 mg, 0.2 mmol.) and Et3N (54.8 μl, 0.4 mmol) were added. The mixture was stirred at room temperature for 30 min. 3-(trifluoromethyl)benzyl amine (57.33 μl, 0.4 mmol) was added to the mixture and stirring continued for 18 h. H2O was added to the mixture and the product extracted with EtOAc, dried over MgSO4 and concentrated. Purification was done by flash chromatography (CH2Cl2/MeOH 98:2→96:4) giving 20.0 mg (12%) of the title compound.

후처리

  1. temperaturethe mixture refluxed for 3.0 days
  2. temperatureThe mixture was cooled
  3. concentrationconcentrated to dryness
  4. stirringstirring
  5. waitcontinued for 18 h
  6. extractionthe product extracted with EtOAc
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated
  9. customPurification

출처 및 근거

ORD 기록
ord-92e0c5ada0b84da7be64a8e86960473f
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08415333B2

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