反应详情

温度

60 °C

To 90% aqueous ethanol (water:ethanol =1:9, v/v), 7 g of (±)-2,8-dimethyl-3-methylene-1-oxa-8-azaspiro[4.5]decane and 5.79 g of L-tartaric acid were added and dissolved by heating at 60° C. The resulting solution was allowed to cool and maintained at about 4° C. for 15 hours. The resulting crystals were collected by filtration and, without drying, recrystallized from 9 ml of 90% aqueous ethanol. This recrystallization procedure was repeated further twice and the crystals obtained were dried under reduced pressure to give 3.22 g of (-)-(S)-2,8-dimethyl-3-methylene-1-oxa-8-azaspiro[4.5]decane L-tartrate monohydrate.

1. dissolutiondissolved
2. temperatureto cool
3. temperaturemaintained at about 4° C. for 15 hours
4. filtrationThe resulting crystals were collected by filtration
5. customwithout drying
6. customrecrystallized from 9 ml of 90% aqueous ethanol
7. customThis recrystallization procedure
8. customthe crystals obtained
9. customwere dried under reduced pressure