1,2-Dibromoethane → HCID 178480304, compound

Participants

Reaction Steps

To 12.9 g of magnesium turnings of 50 ml of tetrahydrofuran, under nitrogen, was added several ml of a solution of 71.4 g of 1-methyl-3-chloromethylpiperidine in about 50 ml of tetrahydrofuran. Reaction was initiated by adding about 0.6 ml of ethylene dibromide. The remaining 3-chloromethylpiperidine solution then was added at a rate sufficient to maintain the reaction mixture at reflux temperature, with the concomitant addition of about 100 ml of tetrahdrofuran. When the addition of the 3-chloromethylpiperidine solution was complete, and additional 150 ml of tetrahydrofuran was added. The reaction mixture was warmed to maintain the reaction, after which the reaction mixture was heated at reflux for 1 hour. The reaction mixture then was cooled to ambient temperature and filtered through glass wool to remove excess magnesium.

Provenance & Evidence