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1-Hydroxybenzotriazole → 3-(R)-Azido-2-(S)-[(4'-ethyl-biphenyl-4-carbonyl)-amino]-butyric acid methyl ester

HRID 422962
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HRID 422962 반응식
CCN=C=NCCCN(C)C.Cl.Cl.[CH3:14][O:15][C:16](=[O:24])[C@@H:17]([NH2:23])[C@H:18]([N:20]=[N+:21]=[N-:22])[CH3:19].C1C=CC2N(O)N=NC=2C=1.[CH2:35]([C:37]1[CH:42]=[CH:41][C:40]([C:43]2[CH:48]=[CH:47][C:46]([C:49](O)=[O:50])=[CH:45][CH:44]=2)=[CH:39][CH:38]=1)[CH3:36].CCN(C(C)C)C(C)C>C(Cl)Cl.CCCCCC.CCOC(C)=O>[CH3:14][O:15][C:16](=[O:24])[C@@H:17]([NH:23][C:49]([C:46]1[CH:45]=[CH:44][C:43]([C:40]2[CH:41]=[CH:42][C:37]([CH2:35][CH3:36])=[CH:38][CH:39]=2)=[CH:48][CH:47]=1)=[O:50])[C@H:18]([N:20]=[N+:21]=[N-:22])[CH3:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 5218014-(4-Ethylphenyl)benzoic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 86643747(2S,3R)-2-amino-3-azido-butyric acid methylester hydrochloride

생성물 1

HCID 59697227
3-(R)-Azido-2-(S)-[(4'-ethyl-biphenyl-4-carbonyl)-amino]-butyric acid methyl ester
수율 67%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 21226206Ethyl acetate hexane용매

실험 절차

A EDC.HCl (249 mg, 1.3 mmol) was added to a stirred colorless solution of azido-Thr-OMe.HCl (4) (195 mg, 1.0 mmol), HOBT (158 mg, 1.0 mmol), 4′-Ethyl-biphenyl-4-carboxylic acid (5) (226 mg, 1.0 mmol) and DIEA (0.44 ml, 2.5 mmol) in DCM (10 ml) at rt under N2. After 24 h, the reaction had reached completion by TLC (Hexane/EtOAc (60:40) (Rf=0.3)) and LCMS. The reaction was evaporated under reduced pressure to a brown tar. The crude product was dissolved in EtOAc (100 ml) and washed with 0.2N aq. HCl (2×50 ml), aq. sat. NaHCO3 (50 ml), brine (50 ml), dried (Na2SO4), filtered and concentrated under reduced pressure to yield a crude brown solid. The crude material was further purified by column chromatography eluting with Hexane/EtOAc (70:30) giving 245 mg (67% yield) of pure product after evaporation and drying in vacuo.

후처리

  1. customThe reaction was evaporated under reduced pressure to a brown tar
  2. dissolutionThe crude product was dissolved in EtOAc (100 ml)
  3. washwashed with 0.2N aq. HCl (2×50 ml), aq. sat. NaHCO3 (50 ml), brine (50 ml)
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customto yield a crude brown solid
  8. customThe crude material was further purified by column chromatography
  9. washeluting with Hexane/EtOAc (70:30)

출처 및 근거

ORD 기록
ord-aa9c558a44a04f948fb0753deb75b8f0
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08101640B2

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