Reaktion #54683

Reaktionsgleichung

2,4-diamino-6-chloropyrimidine

ethanol

peracetic acid

→

2,4-diamino-6-chloro-pyrimidine-3-oxide

Lösungsmittel

acetic acid

—

petroleum ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThis mixture is then cooled down to 6°-8° C. and at this temperature there
2. 2
   workup.ADDITIONare added dropwise within 40 minutes 175 ml
3. 3
   workup.ADDITIONAfter completion of the addition
4. 4
   workup.STIRRINGthe mixture is stirred at 6°-8° C. for a further 30 minutes
5. 5
   workup.WAITThereafter, the mixture is left
6. 6
   Temperaturto warm up to room temperature
7. 7
   workup.STIRRINGstirred at this temperature for 3 hours
8. 8
   workup.STIRRINGthe mixture is stirred for 1 hour
9. 9
   workup.WAITleft
10. 10
    workup.WAITto stand overnight
11. 11
    FiltrationThe separated precipitate is filtered off
12. 12
    Waschenback-washed with 200 ml
13. 13
    Trocknenof petroleum ether and dried under reduced pressure, there

Vorschrift

144.5 G. of 2,4-diamino-6-chloropyrimidine are suspended in 2000 ml. of ethanol. The suspension is warmed to 35° C. while stirring (about 15 minutes), the greater part of the material passing into solution. This mixture is then cooled down to 6°-8° C. and at this temperature there are added dropwise within 40 minutes 175 ml. of 40% peracetic acid in glacial acetic acid. After completion of the addition, the mixture is stirred at 6°-8° C. for a further 30 minutes. Thereafter, the mixture is left to warm up to room temperature, and stirred at this temperature for 3 hours. 2000 Ml. of petroleum ether are added, the mixture is stirred for 1 hour and then left to stand overnight. The separated precipitate is filtered off, back-washed with 200 ml. of petroleum ether and dried under reduced pressure, there being obtained 2,4-diamino-6-chloro-pyrimidine-3-oxide. Recrystallization yields analytically pure product having a melting point of 193° C.

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