Reaktion #1856131

Reaktionsgleichung

water

4-[3-[4-(1-adamantyl)-1-piperazinyl]-2-hydroxypropoxy]benzylcyanide

5-nitroso-2,4,6-triamino-pyrimidine

sodium-(2-ethoxyethoxide)

→

title compound

Ausbeute 84.6%

6-[4-[3-[4-(1-Adamantyl)-1-piperazinyl]-2-hydroxypropoxy]phenyl]-2,4,7-triaminopteridine

Ausbeute 84.6%

Lösungsmittel

2-ethoxyethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturAfter cooling to about 90° C
2. 2
   Temperaturthe mixture was cooled to room temperature
3. 3
   workup.STIRRINGby stirring in an ice-water bath for 30 minutes
4. 4
   SonstigeThe precipitate was collected
5. 5
   Waschenwashed with water and acetonitrile

Vorschrift

A mixture of 4-[3-[4-(1-adamantyl)-1-piperazinyl]-2-hydroxypropoxy]benzylcyanide (3.44 g, 8.4 mmol), 5-nitroso-2,4,6-triamino-pyrimidine (1.08 g, 7.0 mmol) and 0.2N sodium-(2-ethoxyethoxide) in 2-ethoxyethanol (35 ml) was stirred at 120° C. for 30 minutes. After cooling to about 90° C. 100 ml of water was added and the mixture was cooled to room temperature followed by stirring in an ice-water bath for 30 minutes. The precipitate was collected, washed with water and acetonitrile to give the title compound (3.23 g) as a yellow powder, mp. 287°-289° C. (dec.), yield: 84.6%.

Quelle