HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ammonia → 2-(3-Cyanopropyl)-4-dimethylaminomethylpyridine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ammonia | HCID 222 | — |
| Edukt | Sulfuric Acid | HCID 1118 | — |
| Edukt | 4-Cyanobutanoic acid | HCID 38239 | — |
| Edukt | Ammonium Persulfate | HCID 62648 | — |
| Edukt | 4-pyridinemethanamine, N,N-dimethyl- | HCID 264946 | — |
| Katalysator | Silver Nitrate | HCID 24470 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 2-(3-Cyanopropyl)-4-dimethylaminomethylpyridine | HCID 13292607 | 36,9% |
Reaktionsschritte
Ammonium persulphate (54.8 g) in water (150 ml) and 4-cyanobutyric acid (68 g) in water (300 ml) were added separately and simultaneously over 30 minutes to a mixture of 4-dimethylaminomethylpyridine (16.32 g), silver nitrate (4 g), water (200 ml) and concentrated sulphuric acid (25 ml) stirred at 80°. The reaction mixture was stirred at 80° for 1.5 hours, cooled, poured onto crushed ice (400 g) and aqueous ammonia (28% w/w, 200 ml). The solution was extracted with chloroform (900 ml) and the chloroform extracts were washed with dilute sodium hydroxide, dried over magnesium sulphate, and concentrated in vacuo to give 2-(3-cyanopropyl)-4-dimethylaminomethylpyridine (9 g) as a clear oil b.p. 110°-112°/0.1 mm Hg.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04439609 |
| Quelldatensatz | uspto-grants-1984_03 |
| ORD ID | ord-90ca783611704bf0ade04ddab6a76680 |
| Quellennotiz | uspto-grants-1984_03 |