Boron Trichloride → HCID 11172974, compound

Participants

Reaction Steps

To a solution of boron trichloride (1M solution) in dry dichloromethane (7 mL, 7 mmol) cooled to −78° C., was added dropwise over a period of 30 min, a solution of compound 7 (265 mg, 0.5 mmol) in dry dichloromethane (10 mL). Stirring was continued overnight at −20° C. The solvent was removed in vacuo and the residue was coevaporated with dichloromethane (4×20 mL). The residue was neutralized with saturated NaHCO3 (25 mL) and washed with chloroform (15 mL). The aqueous layer was applied to a cation exchange (H+) column and eluted with water to remove salts and then eluted with 1N NH4OH to obtain the desired compound 8 (110 mg, 85%) MS z/e 260(M+H)+.

Provenance & Evidence