HCID 54363480, compound → HCID 13321926, compound

Participants

Reaction Steps

10.0 g (38 millimoles) of 3-(2,3-dihydro-1,1-dioxido-3-oxo-1,2-benzisothiazol-2-yl)-1-cyano-2-methylprop-1-ene (Example 1) were dissolved in 200 ml of ethanol and 100 ml of dimethylformamide, 1 g of palladium on active carbon (10%) was added and hydrogenation was carried out for 12 hours at room temperature and under atmospheric pressure. The mixture was filtered, the filtrate was evaporated down under reduced pressure and the resulting greenish oil was purified by column chromatography (silica gel, mobile phase 85:15 mixture of toluene and methanol) to give 4.8 g (48%) of 3-(2,3-dihydro-1,1-dioxido-3-oxo-1,2-benzisothiazol-2-yl)-1-cyano-2-methylpropane in the form of an oil which slowly crystallized through. Mp 83°-84° C.

Provenance & Evidence