Reaktion #1109182

Reaktionsgleichung

230b

(S)-tert-Butyl 4-(5-(Diphenylmethyleneamino)pyrazin-2-yl)-3-methylpiperazine-1-carboxylate

sodium acetate

hydroxylamine hydrochloride

→

230c

Ausbeute 64.0%

(S)-tert-Butyl 4-(5-Aminopyrazin-2-yl)-3-methylpiperazine-1-carboxylate

Ausbeute 64.0%

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenIt was then concentrated in vacuo
2. 2
   SonstigeThe residue was purified by silica-gel column chromatography
3. 3
   Wascheneluting with dichloromethane/methanol (50:1 to 30:1)

Vorschrift

To a solution of 230b (3.3 g, 7.2 mmol) in methanol (25 mL) were added sodium acetate (708 mg, 8.6 mmol) and hydroxylamine hydrochloride (907 mg, 8.6 mmol). The reaction mixture was stirred for 0.5 h. It was then concentrated in vacuo. The residue was purified by silica-gel column chromatography eluting with dichloromethane/methanol (50:1 to 30:1) to afford 230c as yellow oil (1.35 g, 64%). MS: [M+H]+ 294.3.

Quelle