Lawesson's reagent → HCID 59446284, compound

Participants

Reaction Steps

Lawesson's reagent (134 mg) was added to a toluene (5 ml) solution of Compound 19c (300 mg), and the obtained mixture was stirred while refluxing under heating for 20 minutes. After the mixture was allowed to cool, the solvent was distilled off. The obtained residue was purified by column chromatography (6.25% ethyl acetate/n-hexane). Fractions containing the ester body of Compound 19 were collected and concentrated to dryness. As a result, 246 mg of yellow solid was obtained. The obtained yellow solid was, without further purification, dissolved in ethanol (10 ml), and a 2N sodium hydroxide aqueous solution (2.62 ml) was added thereto in a nitrogen atmosphere. The obtained mixture was stirred under heating at 70° C. for 2 hours. After the reaction was over, the mixture was allowed to cool. A 2N hydrochloric acid aqueous solution was added thereto, and the mixture was separated with ethyl acetate and water. The organic layer was washed once with water and once with a saturated sodium chloride solution, and then dried over anhydrous sodium sulfate. The solvent was distilled off, and as a result, Compound 19 (112 mg, 48%) was obtained as a yellow solid.

Provenance & Evidence