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Triethylamine → (S)-4-(5-(4-isopropyl-2-oxooxazolidin-3-yl)pyrazolo[1,5-a]pyrimidin-3-yl)benzohydrazide

HRID 538999
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HRID 538999 반응식
CCN=C=NCCCN(C)C.[CH:12]([C@H:15]1[CH2:19][O:18][C:17](=[O:20])[N:16]1[C:21]1[CH:26]=[CH:25][N:24]2[N:27]=[CH:28][C:29]([C:30]3[CH:38]=[CH:37][C:33]([C:34](O)=[O:35])=[CH:32][CH:31]=3)=[C:23]2[N:22]=1)([CH3:14])[CH3:13].C1C=CC2N(O)[N:46]=[N:45]C=2C=1.O.O.NN.C(N(CC)CC)C>CN(C=O)C.CCOC(C)=O>[CH:12]([C@H:15]1[CH2:19][O:18][C:17](=[O:20])[N:16]1[C:21]1[CH:26]=[CH:25][N:24]2[N:27]=[CH:28][C:29]([C:30]3[CH:31]=[CH:32][C:33]([C:34]([NH:45][NH2:46])=[O:35])=[CH:37][CH:38]=3)=[C:23]2[N:22]=1)([CH3:14])[CH3:13]
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참가 물질

8

반응물 5

HCID 8471TriethylamineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 24654Hydrazine hydrate (1:1)HCID 27960291-Hydroxybenzotriazole hydrateHCID 67034480(S)-4-(5-(4-isopropyl-2-oxooxazolidin-3-yl)pyrazolo[1,5-a]pyrimidin-3-yl)benzoic acid

생성물 1

HCID 67033928
(S)-4-(5-(4-isopropyl-2-oxooxazolidin-3-yl)pyrazolo[1,5-a]pyrimidin-3-yl)benzohydrazide
수율 64%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매2회HCID 8857Ethyl Acetate용매

실험 절차

EDCI (2.39 g, 12.45 mmol) was added to a mixture of (S)-4-(5-(4-isopropyl-2-oxooxazolidin-3-yl)pyrazolo[1,5-a]pyrimidin-3-yl)benzoic acid (0.76 g, 2.1 mmol) and HOBT-H2O (0.95 g, 6.226 mmol) in DMF (10 mL) at ambient temperature, and the reaction mixture was stirred for 20 minutes at ambient temperature. A solution of hydrazine hydrate (0.31 mL, 6.2 mmol) in DMF and triethylamine (1.5 mL, 10.38 mmol) were added. The resulting mixture was stirred for 1 hour at ambient temperature. The reaction mixture was diluted with EtOAc, washed with aqueous NH4Cl, NaHCO3, and brine, dried over MgSO4, and concentrated under reduced pressure. The crude was purified by silica gel flash column chromatography (0-5% MeOH in dichloromethane) to afford 0.50 g (64%) of (S)-4-(5-(4-isopropyl-2-oxooxazolidin-3-yl)pyrazolo[1,5-a]pyrimidin-3-yl)benzohydrazide. LCMS (APCI+) m/z 381.4 [M+H]+.

후처리

  1. stirringThe resulting mixture was stirred for 1 hour at ambient temperature
  2. washwashed with aqueous NH4Cl, NaHCO3, and brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated under reduced pressure
  5. customThe crude was purified by silica gel flash column chromatography (0-5% MeOH in dichloromethane)

출처 및 근거

ORD 기록
ord-6d6bb08b0f9c40dda515d2373c84fd0e
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08865726B2

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