Methanol → 1-[(5-Chloroisoindol-2-yl)sulfonyl]piperazine

反応式

C([N:8]1[CH2:13][CH2:12][N:11]([S:14]([N:17]2[CH:25]=[C:24]3[C:19]([CH:20]=[CH:21][C:22]([Cl:26])=[CH:23]3)=[CH:18]2)(=[O:16])=[O:15])[CH2:10][CH2:9]1)C1C=CC=CC=1.ClC(OC(Cl)C)=O.CO>ClCCCl>[Cl:26][C:22]1[CH:21]=[CH:20][C:19]2[C:24](=[CH:25][N:17]([S:14]([N:11]3[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]3)(=[O:16])=[O:15])[CH:18]=2)[CH:23]=1

参加物

実験手順

To a solution of 1-benzyl-4-[(5-chloroisoindol-2-yl)sulfonyl]piperazine (222 mg) in 1,2-dichloroethane (20 ml), 1-chloroethyl chloroformate (81 mg) was added under ice cooling. The resulting mixture was stirred for 15 minutes and then heated under reflux for 1 hour. After cooling, anhydrous methanol was added to the residue obtained by distilling off the solvent under reduced pressure. The mixture was heated under reflux for 11 hours. After cooling, the residue obtained by distilling off the solvent under reduced pressure was purified by chromatography on a silica gel column (ethanol:dichloromethane=1:50 to 1:10), whereby the title compound (120 mg, 70%) was obtained.