Reaktion #79083

Reaktionsgleichung

2,4-diamino,5-cyanopyridinium acetate

formic acid

benzylamine

→

7-amino-2-benzylaminopyrido[4,3-d]pyrimidine

Ausbeute 73.3%

Lösungsmittel

water

Water

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturUpon cooling
2. 2
   SonstigeThe liquid is decanted
3. 3
   WaschenThe solid is washed with water
4. 4
   Sonstigerecrystallized from isopropanol (25 mL)
5. 5
   SonstigeAfter drying in a vacuum oven overnight

Vorschrift

A mixture of 2,4-diamino,5-cyanopyridinium acetate (8.78 g, 45 mmol), formic acid (10.66 g, 0.204 mol) and benzylamine (45 mL, 0.41 mol) is heated at 200° C. under N2 for 2 h. Upon cooling, it solidifies. Water (500 mL) is added and the gummy solid/water mixture is stirred for −20 min. at 0° C. The liquid is decanted. The solid is washed with water and then recrystallized from isopropanol (25 mL). After drying in a vacuum oven overnight, 7-amino-2-benzylaminopyrido[4,3-d]pyrimidine (8.29 g, 73%) is obtained as a light yellow solid. 1H NMR (DMSO) δ 9.10 (1H, s), 8.85 (1H, t, J=5.8 Hz), 8.25 (1H, s), 7.21-7.36 (5H, m), 6.46 (2H, brs), 6.35 (1H, s), 4.74 (2H, d, J=6.0 Hz).

Quelle