Lawesson's reagent → HCID 14424293, compound

Participants

Reaction Steps

Under a dry nitrogen atmosphere N-[2-(thien-2-yl)-2-oxoethyl]-4-trifluoromethylbenzamide (5.6 g of the solid from Step D) was added to a stirred suspension of [2,4-bis-(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide (Lawesson's reagent) (3.6 g, 0.0090 mole) in 150 ml of toluene. The resultant mixture was heated at reflux for four hours, then was allowed to cool to room temperature, and was stirred for approximately 18 hours. The mixture was heated at reflux for three hours and then was cooled. The solvent was removed from the mixture by evaporation under reduced pressure, leaving a residue. This residue was purified by column chromatography on silica gel, eluting with methylene chloride:n-hexane (3:1) to yield 2.84 g of 2-(4-trifluoromethylphenyl)-5-thien-2-ylthiazole, as a solid, mp 153.5°-155° C.

Provenance & Evidence