1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 16222146, 화합물

HRID 1717428노트

반응식

HRID 1717428 반응식
[CH:1](/[C:4]1[N:8]([C:9]2[CH:14]=[CH:13][C:12]([C:15]([NH:17][CH2:18][C:19]([F:22])([F:21])[F:20])=[O:16])=[CH:11][CH:10]=2)[N:7]=[N:6][C:5]=1[C:23](O)=[O:24])=[CH:2]\[CH3:3].[CH:26]1([NH2:29])[CH2:28][CH2:27]1.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C>CN(C=O)C.C(OCC)(=O)C.O.C(N(CC)CC)C>[CH:26]1([NH:29][C:23]([C:5]2[N:6]=[N:7][N:8]([C:9]3[CH:14]=[CH:13][C:12]([C:15]([NH:17][CH2:18][C:19]([F:20])([F:21])[F:22])=[O:16])=[CH:11][CH:10]=3)[C:4]=2/[CH:1]=[CH:2]/[CH3:3])=[O:24])[CH2:28][CH2:27]1

참가 물질

9

반응물 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 69828CyclopropylamineHCID 757711-HydroxybenzotriazoleHCID 68515283HCID 68515283, 화합물

생성물 1

HCID 16222146HCID 16222146, 화합물수율 52%

시약·촉매·용매 4

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8471Triethylamine용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 5-[(1E)-prop-1-en-1-yl]-1-(4-{[(2,2,2-trifluoroethyl)amino]carbonyl}phenyl)-1H-1,2,3-triazole-4-carboxylic acid (1.96 g) obtained in Example 1215a) in DMF (22 ml) were successively added cyclopropylamine (0.46 ml), triethylamine (0.92 ml), HOBt (1.01 g) and WSC (1.27 g), and the reaction mixture was stirred at room temperature for 2.5 hr. Water and ethyl acetate were added to the reaction mixture and the organic layer was separated. The organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column (ethyl acetate/hexane=1/1 to ethyl acetate) and recrystallized from ethyl acetate-diisopropyl ether to give the title compound as a white powder (1.13 g, 52%).

후처리

  1. customthe organic layer was separated
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. customthe solvent was evaporated under reduced pressure
  4. customThe residue was purified by silica gel column (ethyl acetate/hexane=1/1 to ethyl acetate)
  5. customrecrystallized from ethyl acetate-diisopropyl ether

출처 및 근거

ORD 기록
ord-d8153be25fdb4657a77f0ee94e6ac9a4
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07803822B2

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