HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Allylamine → N-Allyl-2-iodobenzamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Allylamine | HCID 7853 | — |
| Edukt | 4-Methylmorpholine | HCID 7972 | — |
| Edukt | 2-Iodobenzoyl chloride | HCID 69112 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | N-Allyl-2-iodobenzamide | HCID 2190306 | — |
Reaktionsschritte
470 ml (4.28 mol) of N-methylmorpholine, followed by 224 ml (2.98 mol) of allylamine are added under ice cooling to 750 g (2.81 mol) of 2-iodo-benzoic acid chloride in 7.5 l of acetonitrile, and stirred for 60 min at RT. The precipitate is filtered off and the filtrate concentrated by evaporation on a RE. The residue of evaporation is dissolved in 4 l of EtOAc and 4 l of water, the water phase is separated and extracted twice with EtOAc. The organic phases are washed with water, 0.1 N HCl, water, sat. Na2CO3, water and brine, dried (Na2SO4) and concentrated by evaporation. Stirring of the residue in 2.5 l of hexane and filtering yields 2-iodo-benzoic acid allylamide; m.p. 105-106° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06706731B2 |
| Quelldatensatz | uspto-grants-2004_03 |
| ORD ID | ord-62c7c866bd5f45e0af5784edde849ebc |
| Quellennotiz | uspto-grants-2004_03 |