Triethyloxonium tetrafluoroborate → 1-[(2-Chlorophenyl)carbonyl]-3-(ethyloxy)piperazine
반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]([N:10]1[CH2:15][CH2:14][NH:13][C:12](=[O:16])[CH2:11]1)=[O:9].F[B-](F)(F)F.[CH2:22]([O+](CC)CC)[CH3:23]>ClCCl>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]([N:10]1[CH2:15][CH2:14][NH:13][CH:12]([O:16][CH2:22][CH3:23])[CH2:11]1)=[O:9]참가 물질
4
반응 조건
- 온도
- 25 °C
실험 절차
4-[(2-chlorophenyl)carbonyl]-2-piperazinone (I4) (676 mg, 2.83 mmol) was dissolved in dichloromethane (DCM) (10 mL) and was treated with triethyloxonium tetrafluoroborate (628 mg, 3.31 mmol). The solution was stirred at 25° C. for 16 hr and the solution partitioned between ethyl acetate (25 mL) and saturated sodium bicarbonate solution (25 mL). The aqueous phase was extracted with ethyl acetate (3×25 mL), combined extracts were washed with brine (25 mL), dried over anhydrous sodium sulfate and concentrated to a crude oil in 816 mg that was used in the subsequent step without further purification. Compound was not characterised but used directly in the next step.
후처리
- customthe solution partitioned between ethyl acetate (25 mL) and saturated sodium bicarbonate solution (25 mL)
- extractionThe aqueous phase was extracted with ethyl acetate (3×25 mL)
- washwere washed with brine (25 mL)
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated to a crude oil in 816 mg that
- customwas used in the subsequent step without further purification
출처 및 근거
- ORD 기록
- ord-14bb6c053b484a4e90b40085625e7b2a
- 출처 데이터셋
- uspto-grants-2013_08
- 특허 번호
- US08501946B2
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