反应详情

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°.

1. temperaturecooled
2. customquenched in one liter of cold ether
3. filtrationFiltration
4. customgave a solid crude product, m.p. 79° - 81°
5. customEvaporation of the filtrate and trituration of the residue with cold ether
6. customgive additional crude product
7. extractionThe crude product was continuously extracted from a Soxhlet thimble with ether for 18 hours
8. additionThe solvent pot (not containing
9. customcrystallized product)
10. temperaturewas cooled
11. filtrationthe solid product was filtered