Pyridine → 1-Piperazinecarbonyl chloride, 4-(methylsulfonyl)-
반응식
[Cl:1][C:2](Cl)([O:4]C(=O)OC(Cl)(Cl)Cl)Cl.[CH3:13][S:14]([N:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1)(=[O:16])=[O:15].N1C=CC=CC=1>C(Cl)Cl>[CH3:13][S:14]([N:17]1[CH2:22][CH2:21][N:20]([C:2]([Cl:1])=[O:4])[CH2:19][CH2:18]1)(=[O:16])=[O:15]참가 물질
5
실험 절차
To a stirred solution of carbonic acid ditrichloromethyl ester (triphosgene) (1.81 g, 6.09 mmol) in CH2Cl2 (30 ml) at 0° C., was added a solution of 1-methanesulfonyl-piperazine (2.0 g, 12.2 mmol) and pyridine (1.08 ml, 13.4 mmol) in CH2Cl2 (5 ml) over 30 minutes. The temperature was raised to RT, and stirring was continued over night. The organic phase was washed with H2O, dried over Na2SO4. Purification by flash chromatography (SiO2, EtOAc) yielded 2.20 g (79%) of the title compound as white solid.
후처리
- waitwas continued over night
- washThe organic phase was washed with H2O
- dry with materialdried over Na2SO4
- customPurification by flash chromatography (SiO2, EtOAc)
출처 및 근거
- ORD 기록
- ord-d1e5bebb638444758204fb6e7da5bb21
- 출처 데이터셋
- uspto-grants-2011_02
- 특허 번호
- US07893062B2
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