反应详情

A solution of dimercaptoacetyl boc-serinol (4.1 mmol) in EtOH (20 ml) was treated with 10 ml of aqueous 1 N NaOH at room temperature for 1 h. The mixture was diluted with CH2Cl2 (100 ml) and then an aqueous solution of 0.1 M iodine (4.5 mmol) is added dropwise. The reaction mixture was stirred for 2 hours at room temperature and 1 mmol of Na2S2O3 (1 M aqueous solution) was added to the reaction mixture. The organic phase was separated, washed with water (3×200 mL), dried with magnesium sulfate, and evaporated at room temperature. The crude product was chromatographed on silica gel (200 mL) using a solvent mixture of hexane and ethyl acetate (40:20) as eluent to give 1,2-dithiolane of boc-serinol.

1. customThe organic phase was separated
2. washwashed with water (3×200 mL)
3. dry with materialdried with magnesium sulfate
4. customevaporated at room temperature
5. customThe crude product was chromatographed on silica gel (200 mL)
6. additiona solvent mixture of hexane and ethyl acetate (40:20) as eluent