Ethanamine, 2,2,2-trifluoro- → HCID 86629793、化合物

HRID 1717252ノート

反応式

HRID 1717252 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

HCID 86629793HCID 86629793、化合物収率 100%

試薬・触媒・溶媒 2

HCID 8471Triethylamine溶媒HCID 21891449acetonitrile N,N-dimethylformamide溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-907a1b5b628c4ff8a5d0c39fb278f030
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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