Reaktion #73182

Reaktionsgleichung

3-methyl-7-(2-butin-1-yl)-8-bromoxanthine

potassium carbonate

N-methyl-2-pyrrolidone

2-chloromethyl-3-cyanopyridine

→

1-[(3-Cyanopyridin-2-yl)methyl]-3-methyl-7-(2-butin-1-yl)-8-bromoxanthine

Lösungsmittel

water

—

N-methyl-2-pyrrolidine

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturis cooled to 25° C
2. 2
   FiltrationThe product is filtered off
3. 3
   Waschenwashed with 2 liters of water
4. 4
   Sonstigedried at 70° C. in a drying cabinet under inertization

Vorschrift

202 g (0.68 mol) of 3-methyl-7-(2-butin-1-yl)-8-bromoxanthine, 188.5 g (1.36 mol) of anhydrous potassium carbonate and 1.68 liters of N-methyl-2-pyrrolidone are initially charged in the reactor and heated to 70° C. Subsequently, 119 g (0.75 mol) of 2-chloromethyl-3-cyanopyridine in 240 ml of N-methyl-2-pyrrolidine (NMP) are added dropwise. The reactor contents are stirred at 70° C. for 19 hours. After the reaction has ended, 2.8 liters of water are added to the reaction mixture and it is cooled to 25° C. The product is filtered off, washed with 2 liters of water and dried at 70° C. in a drying cabinet under inertization.

Quelle