Reaktionsgleichung
CO[C:3]1[CH2:8][CH2:7][CH2:6][CH2:5][N:4]=1.[N+:9]([CH3:12])([O-:11])=[O:10]>>[N+:9]([CH:12]=[C:3]1[CH2:8][CH2:7][CH2:6][CH2:5][NH:4]1)([O-:11])=[O:10]Komponenten
3
Versuchsvorschrift
A solution of 33.9 g of (1A) and 36.6 g of nitromethane was refluxed for 3 days, cooled and quenched in one liter of cold ether. Filtration gave a solid crude product, m.p. 79° - 81°. Evaporation of the filtrate and trituration of the residue with cold ether give additional crude product. The crude product was continuously extracted from a Soxhlet thimble with ether for 18 hours, after which time only a small amount of dark oil remained. The solvent pot (not containing crystallized product) was cooled and the solid product was filtered, giving 2-(nitromethylene)piperidine (1B), as a pale yellow solid, m.p.: 80.5°-81°.
Aufarbeitung
- temperaturecooled
- customquenched in one liter of cold ether
- filtrationFiltration
- customgave a solid crude product, m.p. 79° - 81°
- customEvaporation of the filtrate and trituration of the residue with cold ether
- customgive additional crude product
- extractionThe crude product was continuously extracted from a Soxhlet thimble with ether for 18 hours
- additionThe solvent pot (not containing
- customcrystallized product)
- temperaturewas cooled
- filtrationthe solid product was filtered
Quellen und Nachweise
- ORD-Eintrag
- ord-894727a6715849c29050d42b3e41e492
- Quelldatensatz
- uspto-grants-1977_05
- Patentnummer
- US04025634
Verknüpfte Notizen
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