Bis(2-pyridylmethyl)amine → HCID 67404464、化合物

HRID 910249

反応式

HRID 910249 の反応式
[N:1]1[C:2]([C:10]2[CH:15]=[CH:14][C:13]([C:16]3[CH:20]=[CH:19][N:18]([CH2:21][C:22](O)=[O:23])[N:17]=3)=[CH:12][CH:11]=2)=[CH:3][N:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=12.[CH:25]1[CH:30]=[C:29]([CH2:31][NH:32][CH2:33][C:34]2[N:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)[N:28]=[CH:27][CH:26]=1.ON1C2C=CC=CC=2N=N1.Cl.C(N=C=NCCCN(C)C)C>CN(C)C=O.O.C(N(CC)CC)C>[N:28]1[CH:27]=[CH:26][CH:25]=[CH:30][C:29]=1[CH2:31][N:32]([CH2:33][C:34]1[CH:35]=[CH:36][CH:37]=[CH:38][N:39]=1)[C:22](=[O:23])[CH2:21][N:18]1[CH:19]=[CH:20][C:16]([C:13]2[CH:12]=[CH:11][C:10]([C:2]3[N:1]=[C:5]4[CH:6]=[CH:7][CH:8]=[CH:9][N:4]4[CH:3]=3)=[CH:15][CH:14]=2)=[N:17]1

参加物

8

反応物 4

HCID 73759Bis(2-pyridylmethyl)amineHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 67405489HCID 67405489、化合物

生成物 1

HCID 67404464HCID 67404464、化合物収率 72.5%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8471Triethylamine溶媒

実験手順

2-[3-(4-Imidazo[1,2-a]pyridin-2-ylphenyl)-1H-1-pyrazolyl]acetic acid (51 mg), 2,2′-dipicolylamine (32 mg), and 1-hydroxybenzotriazole (27 mg) were dissolved in N,N-dimethylformamide (1 mL), and triethylamine (56 μL) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (38 mg) were added to the solution, followed by stirring at room temperature for 2 hours. Water was added to the reaction mixture, followed by extraction with chloroform and then drying over magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was subjected to flash column chromatography. Fractions eluted by dichloromethane-methanol (20:1) were concentrated under reduced pressure, and the solid was recovered through filtration by use of diethyl ether, to thereby yield the title compound (58 mg).

後処理

  1. extractionfollowed by extraction with chloroform
  2. dry with materialdrying over magnesium sulfate
  3. customThe solvent was evaporated under reduced pressure
  4. washFractions eluted by dichloromethane-methanol (20:1)
  5. concentrationwere concentrated under reduced pressure
  6. filtrationthe solid was recovered through filtration by use of diethyl ether

出典と根拠

ORDレコード
ord-f9236efd8d384e90a53a9a1fa0931a3f
出典データセット
uspto-grants-2011_09
特許番号
US08022075B2

関連ノート

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