[Cl:1][C:2]1[CH:7]=[C:6]([OH:8])[C:5]([Cl:9])=[CH:4][C:3]=1[S:10](Cl)(=O)=O.OS(O)(=O)=O>[Zn].C1(C)C=CC=CC=1>[Cl:9][C:5]1[CH:4]=[C:3]([SH:10])[C:2]([Cl:1])=[CH:7][C:6]=1[OH:8]To a mixture of 2,5-dichloro-4-hydroxy-benzenesulfonyl chloride (1.28 g, 4.92 mmol) and a solution of 25% of H2SO4 (17 mL), Zinc dust (1.64 g, 24.56 mmol) was added slowly at room temperature. The reaction mixture was allowed to stir at 120° C. overnight. The mixture was then cooled at room temperature and toluene was added. The layers were separated and the aqueous phase was dried over, MgSO4 filtered and concentrated in vacuo to give 514 mg (54%) of the title compound as a white solid, which was used in the next reaction without further purification.
Wird geladen…