Ethanol → HCID 178507684, Verbindung

Temperatur

35 °C

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.

1. temperatureThis mixture is then cooled down to 6°-8° C. and at this temperature there
2. additionare added dropwise within 40 minutes 175 ml
3. additionAfter completion of the addition
4. stirringthe mixture is stirred at 6°-8° C. for a further 30 minutes
5. waitThereafter, the mixture is left
6. temperatureto warm up to room temperature
7. stirringstirred at this temperature for 3 hours
8. stirringthe mixture is stirred for 1 hour
9. waitleft
10. waitto stand overnight
11. filtrationThe separated precipitate is filtered off
12. washback-washed with 200 ml
13. dry with materialof petroleum ether and dried under reduced pressure, there

ORD-Eintrag

ord-8e32e366e0bb464a9c23ca4d3634022b

Quelldatensatz

uspto-grants-1979_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04150131