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Diisopropylamine → HCID 178452034, 화합물

HRID 2289053
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HRID 2289053 반응식
C(N(CC)[CH:5]([CH3:7])[CH3:6])(C)C.[N+:10]([O-:13])(O)=[O:11].CC1C=C(C)[N:17]([C:21](N)=[NH:22])N=1.[NH2:24][CH2:25][CH2:26][C:27]([NH:29][C@H:30]1[CH2:34][CH2:33][N:32]([C:35]([O:37][C:38]([CH3:41])([CH3:40])[CH3:39])=[O:36])[CH2:31]1)=[O:28].[CH:42](NC(C)C)(C)[CH3:43].[C:49]([O:52][CH2:53][CH3:54])(=[O:51])C>CN(C=O)C.ClCCl.O1CCCC1.CCOCC>[N+:10]([C:6]1[CH:5]=[CH:7][C:54]([CH2:53][O:52][C:49]([CH:25]([NH:24][C:21]([NH2:22])=[NH:17])[CH2:26][C:27]([NH:29][C@H:30]2[CH2:34][CH2:33][N:32]([C:35]([O:37][C:38]([CH3:41])([CH3:40])[CH3:39])=[O:36])[CH2:31]2)=[O:28])=[O:51])=[CH:43][CH:42]=1)([O-:13])=[O:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 5

HCID 7912DiisopropylamineHCID 8857Ethyl AcetateHCID 81531DiisopropylethylamineHCID 1981863,5-Dimethyl-1H-pyrazole-1-carboxamidine mononitrateHCID 57142019tert-butyl (3S)-3-(3-aminopropanoylamino)-1-pyrrolidinecarboxylate

생성물 1

HCID 178452034HCID 178452034, 화합물

시약·촉매·용매 4

HCID 3283Diethyl Ether용매HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매2회HCID 8028Tetrahydrofuran용매

실험 절차

Under ice cooling, N,N-diisopropylethylamine (961 μl) and 3,5-dimethylpyrazole-1-carboxamidine nitrate (1.11 g) were added to a solution of tert-butyl (3S)-3-(3-aminopropanoylamino)-1-pyrrolidinecarboxylate (1.42 g) in anhydrous N,N'-dimethylformamide (10 ml) and the mixture was stirred overnight at room temperature. The reaction mixture was poured into ether (150 ml) to give an oily precipitate. The precipitate was dissolved in anhydrous dichloromethane:anhydrous tetrahydrofuran=5:2 (70 ml). To the resulting solution, a solution of N-(4-nitrobenzyloxycarbonyl)oxy-5-norbornene-2,3-dicarboxyimide (4.35 g) in anhydrous dichloromethane (35 ml) was added dropwise under ice cooling, followed by the addition of N,N-diisopropylamine (1.90 ml). The resulting mixture was stirred overnight. To the reaction mixture, ethyl acetate was added. The resulting mixture was washed with water and saturated saline, dried over anhydrous magnesium sulfate and concentrated by evaporation under reduced pressure. The residue was suspended in methanol (50 ml). To the suspension, a 1N aqueous sodium hydroxide solution (6 ml) was added under ice cooling, followed by stirring overnight. The reaction mixture was concentrated by evaporation under reduced pressure and the residue was dissolved in ethyl acetate. The resulting solution was washed with water and saturated saline, dried over anhydrous magnesium sulfate and concentrated by evaporation under reduced pressure. The residue was separated by chromatography through a silica gel column (ethyl acetate, ethyl acetate-methanol), whereby 955 mg of the title target compound were obtained.

후처리

  1. customto give an oily precipitate
  2. stirringThe resulting mixture was stirred overnight
  3. washThe resulting mixture was washed with water and saturated saline
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated by evaporation under reduced pressure
  6. additionTo the suspension, a 1N aqueous sodium hydroxide solution (6 ml) was added under ice cooling
  7. stirringby stirring overnight
  8. concentrationThe reaction mixture was concentrated by evaporation under reduced pressure
  9. dissolutionthe residue was dissolved in ethyl acetate
  10. washThe resulting solution was washed with water and saturated saline
  11. dry with materialdried over anhydrous magnesium sulfate
  12. concentrationconcentrated by evaporation under reduced pressure
  13. customThe residue was separated by chromatography through a silica gel column (ethyl acetate, ethyl acetate-methanol), whereby 955 mg of the title target compound
  14. customwere obtained

출처 및 근거

ORD 기록
ord-d40b31db01024e15b02c780a0492d95c
출처 데이터셋
uspto-grants-2000_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06090802

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