Triethylamine → 1-{4-[(ethylamino)carbonyl]-2-(3-phenylpropoxy)phenyl}-1H-1,2,3-triazole-4-carboxamide

HRID 1717344ノート

反応式

HRID 1717344 の反応式
[CH2:1]([NH:3][C:4]([C:6]1[CH:11]=[CH:10][C:9]([N:12]2[CH:16]=[C:15]([C:17]([OH:19])=O)[N:14]=[N:13]2)=[C:8]([O:20][CH2:21][CH2:22][CH2:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH:7]=1)=[O:5])[CH3:2].C1C=CC2N(O)N=[N:36]C=2C=1.N.C(N(CC)CC)C.CCN=C=NCCCN(C)C>CN(C=O)C.O>[CH2:1]([NH:3][C:4]([C:6]1[CH:11]=[CH:10][C:9]([N:12]2[CH:16]=[C:15]([C:17]([NH2:36])=[O:19])[N:14]=[N:13]2)=[C:8]([O:20][CH2:21][CH2:22][CH2:23][C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=2)[CH:7]=1)=[O:5])[CH3:2]

参加物

7

反応物 4

HCID 8471TriethylamineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 1131751H-Benzotriazole, 1-hydroxy-, ammonium salt (1:1)HCID 685163141-{4-[(ethylamino)carbonyl]-2-(3-phenylpropoxy)phenyl}-1H-1,2,3-triazole-4-carboxylic acid

生成物 1

HCID 576651241-{4-[(ethylamino)carbonyl]-2-(3-phenylpropoxy)phenyl}-1H-1,2,3-triazole-4-carboxamide収率 93.1%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 1-{4-[(ethylamino)carbonyl]-2-(3-phenylpropoxy)phenyl}-1H-1,2,3-triazole-4-carboxylic acid (0.14 g) obtained in Example 133e) in DMF (4 ml) were successively added HOBt-NH3 (0.07 g), triethylamine (0.06 ml) and WSC (0.08 g), and the reaction mixture was stirred at room temperature overnight. Water was added to the reaction mixture and the deposited precipitate was collected by filtration, washed with water, and recrystallized from ethanol-water to give the title compound as a white powder (0.13 g, 89%).

後処理

  1. filtrationthe deposited precipitate was collected by filtration
  2. washwashed with water
  3. customrecrystallized from ethanol-water

出典と根拠

ORDレコード
ord-7b44e36e2a2d4ed3b09ce15a93aac05b
出典データセット
uspto-grants-2010_09
特許番号
US07803822B2

反応ノート

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