Hydrazine hydrate (1:1) → N-[1-(5-Oxo-3-phenyl-4,5-dihydro-1,2,4-triazin-6-yl)propyl]cyclopentanecarboxamide

HRID 7547

反応式

HRID 7547 の反応式
Cl.[C:2]1([C:8](=[NH:10])[NH2:9])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.[NH2:12]N.[CH:14]1([C:19]([NH:21][CH:22]([CH2:30][CH3:31])[C:23](=O)[C:24](OCC)=[O:25])=[O:20])[CH2:18][CH2:17][CH2:16][CH2:15]1>C(O)C>[O:25]=[C:24]1[C:23]([CH:22]([NH:21][C:19]([CH:14]2[CH2:18][CH2:17][CH2:16][CH2:15]2)=[O:20])[CH2:30][CH3:31])=[N:12][N:9]=[C:8]([C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[NH:10]1

参加物

5

実験手順

3.5 g (22.3 mmol, 1 equiv.) benzenecarboximidamide hydrochloride are suspended in 10 ml of ethanol and 1.37 g (26.8 mmol, 1.2 equiv.) hydrazine hydrate are added. After stirring at room temperature for 1 hour, 6.28 g (24.6 mmol, 1.1 equiv) of ethyl 3-[(cyclopentylcarbonyl)amino]-2-oxopentanoate (Example 99A), dissolved in 40 ml of ethanol, are added. The reaction mixture is stirred at 70° C. (bath temperature) for 4 hours. The mixture is evaporated to dryness in vacuo and the product is purified by chromatography (flash or column chromatography or preparative HPLC).

後処理

  1. additionare added
  2. stirringThe reaction mixture is stirred at 70° C. (bath temperature) for 4 hours
  3. customThe mixture is evaporated to dryness in vacuo
  4. customthe product is purified by chromatography (flash or column chromatography or preparative HPLC)

出典と根拠

ORDレコード
ord-ac4239c9e35d4f9abbabb31f98870e4d
出典データセット
uspto-grants-2006_08
特許番号
US07087605B2

関連ノート

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