Pyridine → 1-Piperazinecarbonyl chloride, 4-(methylsulfonyl)-
反応式
[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]参加物
5
実験手順
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.
後処理
- waitwas continued over night
- washThe organic phase was washed with H2O
- dry with materialdried over Na2SO4
- customPurification by flash chromatography (SiO2, EtOAc)
出典と根拠
- ORDレコード
- ord-d1e5bebb638444758204fb6e7da5bb21
- 出典データセット
- uspto-grants-2011_02
- 特許番号
- US07893062B2
反応ノート
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