Boron Trichloride → HCID 22062708, compound

Participants

Reaction Conditions

Reaction Steps

Into clean flame dried Ar flushed 500 mL RBF was placed 6.3 g (19 mmol) of 27 and 100 mL of dry DCM and the mixture was cooled to −78° C. 95 mL of BCl3 (1.0 M solution in DCM) was then slowly added to the above solution. After complete addition the cooling bath was removed and the reaction mixture was allowed to warm to room temperature. Stirring was continued for an additional 30 minutes at room temperature after which the reaction was cooled in an ice-water bath and quenched very cautiously!! (as it turns violent) with 100 mL of water. The organic layer was then separated and washed with water, dried over MgSO4 and the solvents evaporated under vacuum. The crude was then purified with combiflash using hexane/ethylacetate as eluent to furnish 4.3 g of 26 in 94% yield.

Provenance & Evidence