Reaktion #2283885

Reaktionsgleichung

N,N-Dimethyl-5-nitro-1H-pyrrolo[2,3-b]pyridin-3-amine

hydrogen

→

N3,N3-dimethyl-1H-pyrrolo[2,3-b]pyridine-3,5-diamine

Ausbeute 40.0%

Lösungsmittel

EtOAc

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe mixture was then filtered through GF/F
2. 2
   Filtrationfilter paper
3. 3
   Einengenthe filtrate was concentrated to a solid
4. 4
   SonstigeThis material was purified by preparative TLC (0.5 mm plate, 10% MeOH/DCM/0.5% NH4OH)

Vorschrift

N,N-Dimethyl-5-nitro-1H-pyrrolo[2,3-b]pyridin-3-amine (50 mg) was taken up in methanol (3 mL) and EtOAc (3 mL). 10% Pd/C (50 mg) was added, and the mixture was hydrogenated under a balloon of hydrogen for one hour. The mixture was then filtered through GF/F filter paper, and the filtrate was concentrated to a solid. This material was purified by preparative TLC (0.5 mm plate, 10% MeOH/DCM/0.5% NH4OH) to give N3,N3-dimethyl-1H-pyrrolo[2,3-b]pyridine-3,5-diamine (17 mg, 40%). (APCI-pos) M+1=177.2.

Quelle