HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → Terbinafine Hydrochloride
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Terbinafine | HCID 1549008 | — |
| Lösungsmittel | Methyl Ethyl Ketone | HCID 6569 | — |
| Produkt | Terbinafine Hydrochloride | HCID 5282481 | 66,5% |
Reaktionsschritte
14.1 g crude terbinafine (39.9 mmol theoretical, example 6) is dissolved in 94 ml methyl ethyl ketone (MEK) and then 3.9 ml (0.0399 mol) of 32% aqueous hydrochloric acid is added dropwise. The resulting suspension is stirred for 30 minutes and then concentrated to a small volume, using a rotavapor to azeotropically distil off the water. The initial volume is restored with chilled MEK. After stirring for 2 hours at 20° C., the precipitate is filtered, washed with 2×11 ml MEK and dried to constant weight under a heat lamp. 8.7 g (66.4% yield) of terbinafine-HCl are obtained as a white solid with purity of 99.3% (HPLC A %).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07838704B2 |
| Quelldatensatz | uspto-grants-2010_11 |
| ORD ID | ord-14c24fa8f1f34365acedab01bdde6c04 |
| Quellennotiz | uspto-grants-2010_11 |