Boron Trichloride → HCID 22062708, compound

Temperature

-78 °C

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.

1. temperatureInto clean flame
2. customdried Ar
3. customflushed 500 mL RBF
4. additionAfter complete addition the cooling bath
5. customwas removed
6. temperatureto warm to room temperature
7. temperatureafter which the reaction was cooled in an ice-water bath
8. customquenched very cautiously
9. customThe organic layer was then separated
10. washwashed with water
11. dry with materialdried over MgSO4
12. customthe solvents evaporated under vacuum
13. customThe crude was then purified with combiflash

ORD record

ord-9f70edad82d84111a902c8c96620fc45

Source dataset

uspto-grants-2010_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07749983B2