Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Toluene | HCID 1140 | — |
| Edukt | Thionyl Chloride | HCID 24386 | — |
| Edukt | 2-Aminomethyl-1-ethylpyrrolidine | HCID 117295 | — |
| Edukt | 3-Bromo-2,6-dimethoxybenzoic acid | HCID 2774744 | — |
| Lösungsmittel | Diethyl Ether | HCID 3283 | — |
| Lösungsmittel | Methyl Ethyl Ketone | HCID 6569 | — |
| Produkt | HCID 15565708 | HCID 15565708 | — |
Reaktionsschritte
30 ml of thionyl chloride is added to 17.6 g (0.067 mol) of 3-bromo-2,6-dimethoxybenzoic acid. The mixture is heated on a steam bath for 30 minutes. To the solution is added 50 ml of toluene. The solvent and excess thionyl chloride is evaporated at reduced pressure. The residue is dissolved in 50 ml of dry methyl ethyl ketone. The solution is added dropwise while stirring to 9.23 g (0.072 mol) of 2-(aminomethyl)-1-ethylpyrrolidine in 50 ml of methyl ethyl ketone. After stirring for 30 minutes at room temperature 150 ml of ethyl ether is added. The obtained precipitate is filtered off, washed with ether and recrystallized twice from ethanol-isopropyl ether. Yield: 21.0 g, m.p. 182°-84° C. (first recrystallization). m.p. 184°-85° C. (second recrystallization).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US04232037 |
|---|
| Quelldatensatz | uspto-grants-1980_11 |
|---|
| ORD ID | ord-26f7e6a3387244f3ba271f5c15ea707f |
|---|
| Quellennotiz | uspto-grants-1980_11 |
|---|