Reaktion #73183

Reaktionsgleichung

diisopropylethylamine

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

3-(phthalimido)piperidine D-tartrate

N-methyl-2-pyrrolidone

→

1-[(3-Cyanopyridin-2-yl)methyl]-3-methyl-7-(2-butin-1-yl)-8-(3-(R)-phthalimidopiperidin-1-yl)-xanthine

Lösungsmittel

water

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeare metered in within 20 minutes
2. 2
   TemperaturSubsequently, the reaction mixture is cooled to 75° C.
3. 3
   Temperaturthe mixture is cooled to 25° C
4. 4
   FiltrationThe product is filtered off
5. 5
   Waschenwashed with 2 liters of water
6. 6
   SonstigeDrying
7. 7
   Sonstigeis effected at 70° C. in a drying cabinet under inertization

Vorschrift

230 g (0.557 mol) of 1-[(3-cyanopyridin-2-yl)methyl]-3-methyl-7-(2-butin-1-yl)-8-bromoxanthine, 318 g (0.835 mol) of 3-(phthalimido)piperidine D-tartrate and 1.15 liters of N-methyl-2-pyrrolidone are initially charged in the reactor. The reactor contents are heated to 140° C. After the temperature has been attained, 478 ml (2.78 mol) of diisopropylethylamine are metered in within 20 minutes and the reaction mixture is subsequently stirred at 140° C. for 2 hours. Subsequently, the reaction mixture is cooled to 75° C. and diluted with 720 ml of methanol. Afterwards, 2.7 liters of water are added at 68-60° C. and the mixture is cooled to 25° C. The product is filtered off and washed with 2 liters of water. Drying is effected at 70° C. in a drying cabinet under inertization.

Quelle