Example 1
To a solution of the SM (2.63 g, 12.5 mmol) in DCM (60 mL) at 0 C was added DMF (0.49 mL, 6.3 mmol) followed by SOBr2 (1.26 mL, 16.3 mmol). The mixture was allowed to warm to RT and stir for 14 h. Cold ether (30 mL) was added and the mixture was cooled to 0 C, causing solids to precipitate out of solution. The solids were collected by filtration and dried on the filter pad to provide the product as an off-white solid. [3.31 g]
[Patent Reference: WO2016014463, page 122, (6.7 MB)]