Reaktion #7643

Reaktionsgleichung

ethyl 3-[(cyclopentylcarbonyl)amino]-2-oxopentanoate

benzenecarboximidamide hydrochloride

hydrazine hydrate

→

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

Lösungsmittel

ethanol

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONare added
2. 2
   workup.STIRRINGThe reaction mixture is stirred at 70° C. (bath temperature) for 4 hours
3. 3
   SonstigeThe mixture is evaporated to dryness in vacuo
4. 4
   Sonstigethe product is purified by chromatography (flash or column chromatography or preparative HPLC)

Vorschrift

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).

Quelle