Reaktion #73178

Reaktionsgleichung

1-[(4-methylquinazolin-2-yl)methyl]-3-methyl-7-(2-butin-1-yl)-8-bromoxanthine

3-(phthalimido)piperidine D-tartrate

diisopropylethylamine

→

1-[(4-Methylquinazolin-2-yl)methyl]-3-methyl-7-(2-butin-1-yl)-8-(3-(R)-phthalimidopiperidin-1-yl)-xanthine

Lösungsmittel

N-methyl-2-pyrrolidone

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeare metered in within 20 minutes
2. 2
   SonstigeThe feed vessel is flushed with 2.5 liters of N-methyl-2-pyrrolidone
3. 3
   Temperaturthe reaction mixture is cooled to 60° C.
4. 4
   workup.ADDITIONdiluted with 80 liters of methanol
5. 5
   workup.STIRRINGThe resulting suspension is stirred at 50° C. for 30 minutes
6. 6
   Temperaturcooled to 23° C.
7. 7
   workup.STIRRINGstirred for a further 30 minutes
8. 8
   Waschenwashed 3 times with 20 liters each time of methanol
9. 9
   SonstigeDrying
10. 10
    Sonstigeis effected at 45° C. in a drying cabinet under inertization

Vorschrift

10.00 kg (22.06 mol) of 1-[(4-methylquinazolin-2-yl)methyl]-3-methyl-7-(2-butin-1-yl)-8-bromoxanthine, 12.59 kg (33.09 mol) of 3-(phthalimido)piperidine D-tartrate and 17.5 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, 11.41 kg (88.24 mol) of diisopropylethylamine are metered in within 20 minutes. The feed vessel is flushed with 2.5 liters of N-methyl-2-pyrrolidone and the reaction mixture is subsequently stirred at 140° C. for 2 hours. After the reaction has ended, the reaction mixture is cooled to 60° C. and diluted with 80 liters of methanol. The resulting suspension is stirred at 50° C. for 30 minutes, then cooled to 23° C. and stirred for a further 30 minutes. Subsequently, the product is centrifuged off and washed 3 times with 20 liters each time of methanol. Drying is effected at 45° C. in a drying cabinet under inertization.

Quelle