HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 2-Hydroxy-3-methyl-2-(trifluoromethyl)butan-1-aminium chloride
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | 1,1,1-Trifluoro-3-methyl-2-(nitromethyl)butan-2-ol | HCID 86657673 | — |
| Katalysator | Palladium | HCID 23938 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | 2-Hydroxy-3-methyl-2-(trifluoromethyl)butan-1-aminium chloride | HCID 86657674 | — |
Reaktionsschritte
To a solution of 1,1,1-trifluoro-3-methyl-2-(nitromethyl)butan-2-ol (753 mg, 3.74 mmol) in EtOH (10 ml) in a 25 ml medium pressure glass hydrogenation vessel under N2, 10% Pd on carbon (39.8 mg, 0.374 mmol) was added. The vessel was flushed with N2, followed by H2 (22.64 mg, 11.23 mmol) at 5 bar pressure and stirred at RT for 6 days. The mixture was filtered through Celite® and washed through with EtOH(30 ml), followed by DCM (10 ml). The filtrate was concentrated under vacuum to give a colourless oil. The crude product was taken up in methanol (20 ml) and treated with a 1.25M HCl in methanol solution. The resulting colourless solution was stirred at RT for 1 hour and concentrated under vacuum to afford the title compound;
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08247436B2 |
| Quelldatensatz | uspto-grants-2012_08 |
| ORD ID | ord-d7e91a844e5f4fffaca39eb5963c35b6 |
| Quellennotiz | uspto-grants-2012_08 |