Réaction #62990
ord-50a24f73a84448bdaee945495527e333
Équation de réaction
Réactifs
Aucun
Solvants
Conditions de réaction
Conditions détaillées
See reaction.notes.procedure_details.
Traitement
- 1Autrewas reacted at 70° C. in a sealed tube for 20 hours
- 2Températureto cool down
- 3Concentrationthe reaction mixture was concentrated under reduced pressure
- 4workup.ADDITIONThe residue was added with ether
- 5workup.ADDITIONfollowed by a further addition of 10 g of ground sodium hydroxide
- 6FiltrationThe insoluble material was filtered off
- 7Concentrationthe filtrate was concentrated under the atmospheric pressure
- 8workup.DISTILLATIONThe residue was distilled under reduced pressure
- 9Autreto give 4.5 g of a fraction at 80° C./18 Torr (yield: 73%)
Mode opératoire
A solution of 8.0 g of N-(2-chloroethyl)piperidine hydrochloride and 0.5 g of sodium iodide in 60 ml of methanol which contained 40% of methylamine was reacted at 70° C. in a sealed tube for 20 hours. After allowing the reaction mixture to cool down, the reaction mixture was concentrated under reduced pressure. The residue was added with ether, followed by a further addition of 10 g of ground sodium hydroxide. The resulting mixture was stirred for 2 hours. The insoluble material was filtered off and the filtrate was concentrated under the atmospheric pressure. The residue was distilled under reduced pressure to give 4.5 g of a fraction at 80° C./18 Torr (yield: 73%).