Ethanamine, 2,2,2-trifluoro- → HCID 86629793, 화합물

HRID 1717252노트

반응식

HRID 1717252 반응식
[N:1]([C:4]1[CH:12]=[CH:11][C:7]([C:8]([OH:10])=O)=[CH:6][CH:5]=1)=[N+:2]=[N-:3].[F:13][C:14]([F:18])([F:17])[CH2:15][NH2:16].C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C>C(#N)C.CN(C=O)C.C(N(CC)CC)C>[N:1]([C:4]1[CH:5]=[CH:6][C:7]([C:8]([NH:16][CH2:15][C:14]([F:18])([F:17])[F:13])=[O:10])=[CH:11][CH:12]=1)=[N+:2]=[N-:3]

참가 물질

7

반응물 4

HCID 9773Ethanamine, 2,2,2-trifluoro-HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 30341844-Azidobenzoic acid

생성물 1

HCID 86629793HCID 86629793, 화합물수율 100%

시약·촉매·용매 2

HCID 8471Triethylamine용매HCID 21891449acetonitrile N,N-dimethylformamide용매

실험 절차

To a solution of 4-azidobenzoic acid (0.65 g) in acetonitrile-DMF (2:1, 15 ml) were successively added 2,2,2-trifluoroethanamine (0.38 ml), triethylamine (0.67 ml), HOBt (0.79 g) and WSC (0.92 g), and the reaction mixture was stirred overnight at room temperature. The solvent was evaporated under reduced pressure, and the residue was dissolved in ethyl acetate and washed with saturated aqueous sodium hydrogen carbonate solution. The organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure to give the title compound as a white powder (0.98 g, 100%).

후처리

  1. customThe solvent was evaporated under reduced pressure
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washwashed with saturated aqueous sodium hydrogen carbonate solution
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-907a1b5b628c4ff8a5d0c39fb278f030
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07803822B2

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