Reaktion #1068697

Reaktionsgleichung

2,4-Diamino-5-(4-chloro-3-nitro phenyl)-6-ethylpyrimidine

methylamine

methylamine

→

2,4-Diamino-5-(4-methylamino-3-nitrophenyl)-6-ethylpyrimidine

Ausbeute 92.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe consumption of starting material
2. 2
   TemperaturAfter cooling
3. 3
   Sonstigedilution with water, the crystalline product was collected
4. 4
   Sonstigerecrystallized from aqueous DMF

Vorschrift

A suspension of 2,4-Diamino-5-(4-chloro-3-nitro phenyl)-6-ethylpyrimidine (nitropyrimethamine) (10 g) in aqueous methylamine solution (40%; 200 ml) was refluxed for 48 hours with the further addition of methylamine solution (100 ml) after 24 hours and 36 hours. An orange colour slowly developed and the consumption of starting material was monitored by t.l.c. After cooling and dilution with water, the crystalline product was collected and recrystallized from aqueous DMF to yield orange prisms of 2,4-Diamino-5-(4-methylamino-3-nitrophenyl)-6-ethylpyrimidine (9.0 g. 92%), m.p. 262°-265° C. (Elemental analysis: C, 53.9; H, 5.9; N, 29.3%; calculated: C, 54.2; H, 5.6; N, 29.2%).

Quelle