1-Chloroethyl chloroformate → 1-(Benzothiophen-2-yl)piperazine hydrochloride
반응식
C([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[S:15][C:16]3[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=3[CH:18]=2)[CH2:10][CH2:9]1)C1C=CC=CC=1.[Cl:23]C(OC(Cl)=O)C>ClCCl>[ClH:23].[S:15]1[C:16]2[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=2[CH:18]=[C:14]1[N:11]1[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1참가 물질
4
실험 절차
To a solution of 1-benzyl-4-(benzothiophen-2-yl)piperazine (1.5 g, 4.9 mmol) in anhydrous dichloromethane (20 ml) at 0° C. under nitrogen was added 1-chloroethylchloroformate (0.68 ml, 6.37 mmol). The mixture was allowed to warm to room temperature, stirred for 1h and concentrated in vacuo. The crude residue was dissolved in methanol (10 ml) and heated to reflux for 30 minutes, left to cool and the title compound collected by filtration (0.6 g), m.p. 240° C. (dec.).
후처리
- concentrationconcentrated in vacuo
- dissolutionThe crude residue was dissolved in methanol (10 ml)
- temperatureheated
- temperatureto reflux for 30 minutes
- waitleft
- temperatureto cool
- filtrationthe title compound collected by filtration (0.6 g), m.p. 240° C. (dec.)
출처 및 근거
- ORD 기록
- ord-34b4b5ed36e84e4e92d41a459c677a66
- 출처 데이터셋
- uspto-grants-1995_07
- 특허 번호
- US05432177
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