Tin tetrachloride → HCID 11036671, compound

Participants

Reaction Conditions

Reaction Steps

The compound prepared in Example C4 (1.39 g, 2.43 mmol) was dissolved in anhydrous methylene chloride (30 ml) under an argon atmosphere. The solution was cooled to −78° C., and tin(IV) chloride (0.3 ml, 2.56 mmol) was dropwise added to the cooled solution. The reaction solution was stirred for one hr, tin(IV) chloride (0.6 ml, 5.12 mmol) was again dropwise added to the reaction solution, and the mixture was stirred for additional 2 hr. After the completion of the reaction, an aqueous sodium hydrogencarbonate solution was added thereto, and the temperature of the mixture was raised to room temperature, followed by separation. The organic layer was concentrated under reduced pressure, and the concentrate was then purified by column chromatographic separation on silica gel (toluene:ether=15:1) to give the title compound (0.87 g,91%).

Provenance & Evidence