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

HRID 1717344노트

반응식

HRID 1717344 반응식
[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]

참가 물질

7

반응물 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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-7b44e36e2a2d4ed3b09ce15a93aac05b
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07803822B2

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