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

HRID 1961466
ノート
印刷プレビュー

反応式

HRID 1961466 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 7

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-92e0c5ada0b84da7be64a8e86960473f
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08415333B2

反応ノート

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