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

HRID 7547

반응식

HRID 7547 반응식
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

참가 물질

5

반응물 3

HCID 24654Hydrazine hydrate (1:1)HCID 80289Benzamidine, hydrochlorideHCID 21991319Ethyl 3-[(cyclopentylcarbonyl)amino]-2-oxopentanoate

생성물 1

HCID 135752529N-[1-(5-Oxo-3-phenyl-4,5-dihydro-1,2,4-triazin-6-yl)propyl]cyclopentanecarboxamide

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-ac4239c9e35d4f9abbabb31f98870e4d
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07087605B2

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