Sulfuric Acid → HCID 86718261, compound

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Reaction Steps

In 2 ml of toluene, 50 mg of Compound 13-1 synthesized in Production Example 26 was dissolved. To the solution thus obtained, 0.06 ml of triethylamine was added, and the resulting mixture solution was then cooled. To the solution thus cooled, 0.02 ml of thionyl chloride was added, and the resulting mixture solution was stirred for 1 hour while being allowed to reach room temperature. After the reaction, triethylamine hydrochloride generated was removed by filtration from the reaction solution, and the solvent was then distilled away under a reduced pressure to obtain 73 mg of crude product. To the crude product, 2 ml of tetrahydrofuran, 0.05 ml of triethylamine, and 0.05 ml of methanol were added, and the resulting mixture was stirred at room temperature for 0.5 hour. After the reaction, an aqueous solution of diluted sulphuric acid was added to the reaction solution thus obtained, and extraction with ethyl acetate was then carried out. The organic layer was washed with saturated brine and then dried over anhydrous sodium sulfate. The solvent was distilled away under a reduced pressure to obtain 58 mg of Compound 7-1.

Provenance & Evidence