반응 #1328673

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).

출처