Hydrochloric Acid → 2-Hydroxy-3-methyl-2-(trifluoromethyl)butan-1-aminium chloride

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;

1. customThe vessel was flushed with N2
2. filtrationThe mixture was filtered through Celite®
3. washwashed through with EtOH(30 ml)
4. concentrationThe filtrate was concentrated under vacuum
5. customto give a colourless oil
6. stirringThe resulting colourless solution was stirred at RT for 1 hour
7. concentrationconcentrated under vacuum

ORD-Eintrag

ord-d7e91a844e5f4fffaca39eb5963c35b6

Quelldatensatz

uspto-grants-2012_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08247436B2