1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 68516290、化合物

HRID 1717229ノート

反応式

HRID 1717229 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([N:10]2[C:14]([CH2:15][CH2:16][CH3:17])=[C:13]([C:18]([OH:20])=O)[N:12]=[N:11]2)=[CH:6][CH:5]=1)([O-:3])=[O:2].[CH:21]1([NH2:24])[CH2:23][CH2:22]1.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C>C(#N)C>[CH:21]1([NH:24][C:18]([C:13]2[N:12]=[N:11][N:10]([C:7]3[CH:6]=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:9][CH:8]=3)[C:14]=2[CH2:15][CH2:16][CH3:17])=[O:20])[CH2:23][CH2:22]1

参加物

6

反応物 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 69828CyclopropylamineHCID 757711-HydroxybenzotriazoleHCID 433810581-(4-nitrophenyl)-5-propyl-1H-1,2,3-triazole-4-carboxylic acid

生成物 1

HCID 68516290HCID 68516290、化合物収率 82%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a solution of 1-(4-nitrophenyl)-5-propyl-1H-1,2,3-triazole-4-carboxylic acid (1.38 g) obtained in Example 1b) in acetonitrile (50 ml) were successively added cyclopropylamine (0.38 ml), HOBt (0.84 g) and WSC (1.05 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 aqueous sodium hydrogen carbonate solution. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column (ethyl acetate/hexane=1/1) to give the title compound as a pale-yellow solid (1.29 g, 82%).

後処理

  1. customThe solvent was evaporated under reduced pressure
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washwashed with aqueous sodium hydrogen carbonate solution
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  5. customthe solvent was evaporated under reduced pressure
  6. customThe residue was purified by silica gel column (ethyl acetate/hexane=1/1)

出典と根拠

ORDレコード
ord-8fb3a997258e419b890d8cc877dd3e65
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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