Boron tribromide → HCID 20042555, compound

Participants

Reaction Steps

1 g of the product of Step C in 100 ml of methylene chloride was cooled to 0°/+5° C. and over 5 minutes, 24 ml of an M solution of boron tribromide in methylene chloride were added dropwise. After stirring for 4 hours at ambient temperature and then cooling to 0° C., 50 ml of methanol were added slowly and the solvents were eliminated under reduced pressure. The residue was taken up in methanol and filtered to obtain 1.05 g of the expected product. 0.75 g of this product were purified by chromatography on silica (eluent: methylene chloride-methanol-triethylamine 8-1-1) to obtain 0.36 g of pure product which was crystallized from methanol.

Provenance & Evidence