반응 #477187

반응 방정식

methanol

triethylamine

1-(4-Methoxyphenyl)piperazine dihydrochloride

3-chloropropionyl chloride

→

compound

수율 89.3%

3-chloro-1-(4-(4-methoxyphenyl)piperazin-1-yl)propan-1-one

수율 89.3%

용매

methylene chloride

반응 조건

후처리

1. 1
   workup.DISSOLUTIONdissolving
2. 2
   workup.STIRRINGthe reaction solution was stirred at room temperature for 1 hour
3. 3
   추출the reaction solution was extracted with methylene chloride
4. 4
   기타The organic layer was dried with desiccant and
5. 5
   여과then filtered
6. 6
   농축The filtrate was concentrated
7. 7
   기타purified by column chromatography (EtOAc/hexane, 4:1)

실험 절차

1-(4-Methoxyphenyl)piperazine dihydrochloride (1.85 g, 6.976 mmol) was dissolved in methylene chloride. After adding triethylamine (1.9 mL, 13.952 mmol) dropwise at 0° C. and then dissolving, the mixture was stirred for 30 minutes. After adding 3-chloropropionyl chloride (0.67 mL, 6.976 mmol), the reaction solution was stirred at room temperature for 1 hour. After adding methanol, the reaction solution was extracted with methylene chloride. The organic layer was dried with desiccant and then filtered. The filtrate was concentrated and purified by column chromatography (EtOAc/hexane, 4:1). A target compound (1.76 g, 6.224 mmol, 89.3%) was yielded as white solid.

출처