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General procedure for the preparation of disulfides: To the stirred solution of thiols (1 mmol) in dichloromethane (5 ml), NBS (0.5 mmol) was added. The resulting mixture was stirred at room temperature by the time indicated in Table 1. The progress of the reaction was monitored by TLC. After the completion of the reaction, CH2Cl2 (10 ml) was added and the mixture was washed successively with water (2 × 20 mL). The organic layer was separated and dried (Na2SO4). Evaporation of the solvent under reduced pressure gave almost pure product. Further purification was achieved by column chromatography on silica gel or recrystallization from EtOAc-hexane to give pure product in good to excellent yield (Table 1). The products were characterized by comparison of spectral data with those of authentic samples
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General procedure for the preparation of disulfides: To the stirred solution of thiols (1 mmol) in dichloromethane (5 ml), NBS (0.5 mmol) was added. The resulting mixture was stirred at room temperature by the time indicated in Table 1. The progress of the reaction was monitored by TLC. After the completion of the reaction, CH2Cl2 (10 ml) was added and the mixture was washed successively with water (2 × 20 mL). The organic layer was separated and dried (Na2SO4). Evaporation of the solvent under reduced pressure gave almost pure product. Further purification was achieved by column chromatography on silica gel or recrystallization from EtOAc-hexane to give pure product in good to excellent yield (Table 1). The products were characterized by comparison of spectral data with those of authentic samples.
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