Lawesson's reagent → HCID 86668498, compound

Participants

Reaction Conditions

Reaction Steps

A solution of the (RS)-5-(3-bromo-4-fluoro-phenyl)-5-methyl-morpholin-3-one (intermediate X-4) (265 mg, 0.9 mmol) in tetrahydrofuran (5.3 ml) was treated with 2,4-bis(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane-2,4-disulfide (Lawesson's reagent) (380 mg, 0.9 mmol). After 2.5 hours stirring at 70° C. the reaction mixture was evaporated at reduced pressure. The crude product was purified by chromatography on silica gel using a gradient of heptane/ethyl acetate=100/0 to 0/100 as the eluent. The (RS)-5-(3-bromo-4-fluoro-phenyl)-5-methyl-morpholin-3-thione was obtained as a light yellow gum (262 mg, 94% of theory). MS (ISP): m/z=302.2 [M−H]−, 304.1 [M+2−H]−.

Provenance & Evidence