反应详情

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.

1. customReaction
2. temperatureto maintain the reaction mixture
3. temperatureat reflux temperature
4. additionwith the concomitant addition of about 100 ml of tetrahdrofuran
5. temperatureThe reaction mixture was warmed
6. temperatureto maintain
7. customthe reaction
8. temperatureafter which the reaction mixture was heated
9. temperatureat reflux for 1 hour
10. filtrationfiltered through glass wool
11. customto remove excess magnesium