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

HRID 538999
ノート
印刷プレビュー

反応式

HRID 538999 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

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]+.

後処理

  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)

出典と根拠

ORDレコード
ord-6d6bb08b0f9c40dda515d2373c84fd0e
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08865726B2

反応ノート

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