[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([SH:8])=[CH:4][CH:3]=1.[H-].[Na+].CS(O[CH2:16][CH2:17][CH2:18][NH:19][C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])(=O)=O>CN(C=O)C.CCOC(C)=O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][CH2:16][CH2:17][CH2:18][NH:19][C:20](=[O:21])[O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[CH:4][CH:3]=1A solution of 4-chlorothiophenol (91 mg) in 6 mL of DMF was cooled to 0° C. under N2. Sodium hydride (60%, 30 mg) was added and the reaction stirred for 30 minutes. The product from Step A above in 3 mL of DMF was added and the reaction allowed to warm to room temperature while stirring overnight. This was diluted with EtOAc, washed with saturated NaHCO3 and brine and dried over Na2SO4. Concentrating in vacuo gave the titled compound. ESI+ MS: 202 [MH-Boc]+.
Wird geladen…