Dichloromethane → HCID 15491039, compound

Participants

Reaction Conditions

Reaction Steps

To the BFAA methyl ester from Step 1 (assumed 1× mole fraction) was added p-anisoyl chloride (approximately 1.08 parts by weight; 1.1× mole fraction), followed by methylene chloride (approximately 3.11 parts by weight). The mixture was stirred and cooled to about 0-5° C. Tin(IV) chloride (approximately 1.46 parts by weight) was added while controlling the batch temperature below about 10° C. The reaction was stirred at about 0-10° C. for about 3 hours then was warmed and stirred at about 20-25° C. for several hours. Methylene chloride was added and the reaction was cooled and quenched with 4% aqueous hydrochloric acid while controlling the temperature to below about 10° C. The organic layer was separated and washed with water. The organic layer was concentrated under vacuum and dried by distillation of more methylene chloride. The resulting product was dissolved in methylene chloride and transferred to a clean vessel.

Provenance & Evidence