Reaktion #79868

Reaktionsgleichung

trans-4-chloro-5-iodo-7-[4-(4-methylpiperazino)cyclohexyl]-7H-pyrrolo[2,3-d]pyrimidine

ammonium hydroxide

→

trans-5-iodo-7-[4-(4-methylpiperazino)cyclohexyl]-7H-pyrrolo[2,3-d]pyrimidin-4-amine hydrochloride

Lösungsmittel

1,4-dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture is cooled

Vorschrift

A mixture of trans-4-chloro-5-iodo-7-[4-(4-methylpiperazino)cyclohexyl]-7H-pyrrolo[2,3-d]pyrimidine (750 mg, 1.63 mmol) and 1,4-dioxane (10 mL) and 30% aqueous ammonium hydroxide (10 mL) was heated at 120° C. in a sealed tube for 18 hours. The mixture is cooled and lyophilized to give trans-5-iodo-7-[4-(4-methylpiperazino)cyclohexyl]-7H-pyrrolo[2,3-d]pyrimidin-4-amine hydrochloride (750 mg, quantitative): 1H NMR (DMSO-d6, 400 MHz) δ 10.2 (bs, 1H), 8.08(s, 1H), 7.53(s, 1H), 6.59(bs, 2H), 4.50(m, 1H), 2.5-3.2 (m, 9H), 2.51(s, 3H), 1.8-2.0(m, 6H), 1.46 (m, 2H); MS MH+441.2; RP-HPLC (Hypersil HS, 5 μm, 100 A 4.6×250 mm; 25%-100% acetonitrile—0.05 M ammonium acetate over 10 min, 1 ml/min) tr 3.85 min.

Quelle