Reaktion #2325

Reaktionsgleichung

Charcoal

product

4-acetylamino-1-benzylpiperidine

hydrochloric acid

hydrogen

→

4-acetylaminopiperidine hydrochloride

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigehydrogenated at room temperature
2. 2
   Filtrationthen filtered through diatomaceous earth
3. 3
   Sonstigethe filtrate evaporated to dryness

Vorschrift

10% w/w Palladium on charcoal (1.5 g) was added to a solution of the product from step (i) (10.0 g), 1 molar hydrochloric acid (21.5 ml) and methanol (150 ml) and the mixture hydrogenated at room temperature and pressure until the theoretical amount of hydrogen had been taken up. Charcoal was added, the mixture stirred for 1 hour then filtered through diatomaceous earth and the filtrate evaporated to dryness giving 4-acetylaminopiperidine hydrochloride, 8.64 g, as a sticky foam: NMR (CDCl3 +d6DMSO). δ 9,72(1H,b), 9.02(1H,b), 7.40(1H,bd), 3.87(1H,m), 3.30(2H,m), 2.81(2H,m), 1.86(4H,m), 1.80(3H,s); m/e 143 (M+H)+.

Quelle