Water → HCID 136386389, compound

Participants

Reaction Steps

To a solution of the compound obtained in Example 14 (600 mg) in methylene chloride (20 ml) was added titanium tetrachloride (1.1 g) while cooling with ice. After stirring for 2 hours at room temperature followed by addition of water (10 ml), the stirring was continued for further 15 minutes. After discontinuing the stirring, the aqueous layer was isolated, and neutralized with saturated aqueous sodium bicarbonate, and then extracted with ethyl acetate-tetrahydrofurane (3:1, v/v). The extracted organic layer was washed with water, dried (MgSO4) and then the solvent was distilled off to obtain the title compound (305 mg, 62%). The product was recrystallized from dimethylformamide-water. A colorless prism crystal. M.p. 286 to 287° C.

Provenance & Evidence