반응 #1121732
ord-bb014b7be2f148b68e646b6bc65a50a2
반응 방정식
ethyl 4-bromobutanoate
1-methylpiperazine
K2CO3
→
ethyl 4-(4-methylpiperzin-1-yl)butanoate
수율 96.0%
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도was refluxed for 18 h
- 2농축before concentrated in vacuo
- 3기타The organic layer was then separated
- 4추출the aqueous layer was extracted with dichloromethane (DCM, 3×150 mL)
- 5세척The combined organic extracts were washed with water (150 mL)
- 6건조dried (Na2SO4)
- 7농축concentrated in vacuo
실험 절차
A mixture of ethyl 4-bromobutanoate (5.75 g, 29.5 mmol; Aldrich No. 167118) and 1-methylpiperazine (3.55 mL, 32.0 mmol; Aldrich No. 130001) and anhydrous K2CO3 (4.5 g, 32.5 mmol; Fisher No. P208) in acetonitrile (MeCN, 150 mL) was refluxed for 18 h before concentrated in vacuo. The organic layer was then separated and the aqueous layer was extracted with dichloromethane (DCM, 3×150 mL). The combined organic extracts were washed with water (150 mL), dried (Na2SO4), and concentrated in vacuo to give ethyl 4-(4-methylpiperzin-1-yl)butanoate (6.01 g, 96%) as a yellow oil.