[CH3:1][C:2]1[NH:3][CH:4]=[CH:5][C:6]=1[C:7]([O:9][CH2:10][CH3:11])=[O:8].[H-].[Na+].[N:14]1([S:20](Cl)(=[O:22])=[O:21])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1>CN(C=O)C.CC(=O)OCC>[CH3:1][C:2]1[N:3]([S:20]([N:14]2[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)(=[O:22])=[O:21])[CH:4]=[CH:5][C:6]=1[C:7]([O:9][CH2:10][CH3:11])=[O:8]To a solution of ethyl 2-methyl-1H-pyrrole-3-carboxylate (3.06 g, 20 mmol) in dry DMF (40 mL) was added NaH (0.96 mg, 24 mmol) in portions and the mixture was stirred at rt for 30 min. Then a solution of piperidine-1-sulfonyl chloride (4.4 g, 24 mmol) in dry DMF (10 mL) was added and the resulting mixture was stirred overnight, diluted with EA, washed with water and brine, dried over Na2SO4, concentrated and purified by CC (PE/EA=1/0 to 10/1) to give compound 4a (4.77 g, 78%).
불러오는 중…