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

HRID 900548
ノート
印刷プレビュー

反応式

HRID 900548 の反応式
CC[N:3]=C=NCCCN(C)C.Cl.C1C=[CH:15][C:16]2[N:21](O)[N:20]=[N:19]C=2C=1.[CH2:23]([C:25]1[CH:30]=[CH:29][C:28]([C:31]2[CH:36]=[CH:35][C:34]([C:37]([OH:39])=O)=[CH:33][CH:32]=2)=[CH:27][CH:26]=1)[CH3:24].CCN(C(C)C)C(C)C.CCCCCC.C[CH2:56][O:57][C:58]([CH3:60])=[O:59]>C(Cl)Cl>[CH3:56][O:57][C:58](=[O:59])[C@@H:60]([NH:3][C:37]([C:34]1[CH:33]=[CH:32][C:31]([C:28]2[CH:27]=[CH:26][C:25]([CH2:23][CH3:24])=[CH:30][CH:29]=2)=[CH:36][CH:35]=1)=[O:39])[C@H:16]([N:21]=[N+:20]=[N-:19])[CH3:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 5218014-(4-Ethylphenyl)benzoic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 21226206Ethyl acetate hexane

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-34dc51a37d29403e980404e239f71541
出典データセット
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07358359B2

反応ノート

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