반응 #7635

반응 방정식

3-bromobenzenecarboximidamide hydrochloride

compound

Ethyl 3-(acetylamino)-2-oxopentanoate

hydrazine hydrate

→

N-{1-[3-(3-Bromophenyl)-5-oxo-4,5-dihydro-1,2,4-triazin-6-yl]propyl}acetamide

용매

ethanol

ethanol

반응 조건

후처리

1. 1
   workup.ADDITIONare added
2. 2
   workup.STIRRINGThe reaction mixture is stirred at 80° C. (bath temperature) for 4 hours
3. 3
   workup.WAITat room temperature over night
4. 4
   기타The mixture is evaporated to dryness in vacuo
5. 5
   기타the product is purified by chromatography (flash or column chromatography or preparative HPLC)

실험 절차

2.02 (8.6 mmol, 1 equiv.) 3-bromobenzenecarboximidamide hydrochloride are suspended in 50 ml of ethanol and 1.47 g (10.2 mmol, 1.2 equiv.) hydrazine hydrate are added. After stirring at room temperature for 1 hour, 2.59 g (13 mmol, 1.5 equiv) of the compound of Example 2A, dissolved in 10 ml of ethanol, are added. The reaction mixture is stirred at 80° C. (bath temperature) for 4 hours and then at room temperature over night. The mixture is evaporated to dryness in vacuo and the product is purified by chromatography (flash or column chromatography or preparative HPLC).

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