Thionyl Chloride → 2-Azidomethylphenylacetyl Chloride

Beteiligte Stoffe

Reaktionsschritte

2-Azidomethylphenylacetic acid (19.1 g., 0.1 mole) was dissolved in 800 ml. of methylene chloride. To this solution was added slowly thionyl chloride (26 g., 0.2 mole) and 0.5 ml. of dimethylformamide as catalyst. The reaction mixture was heated at reflux temperature under nitrogen atmosphere for 1 hour. The methylene chloride solution was concentrated with the aid of vacuum and the residue oil (checked by IR spectroscopy-carboxyl 1800 cm-1 and azido group at 2010 cm-1) was picked up in 100 ml. of acetone and placed into a dropping funnel for use directly in the subsequent acylation reaction.

Herkunft & Nachweise