1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 68516290, 화합물

HRID 1717229노트

반응식

HRID 1717229 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 68516290HCID 68516290, 화합물수율 82%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-8fb3a997258e419b890d8cc877dd3e65
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07803822B2

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