Ethanol → HCID 178507684, compound

Temperature

35 °C

144.5 g. of 2,4-diamino-6-chloropyrimidine are suspended in 2000 ml. of ethanol. While stirring, the suspension is warmed to 35° C. (about 15 minutes), the greater part of the substance passing into solution. The mixture is then cooled to 6°-8° C. and, at this temperature, there are added dropwise within the course of 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. The mixture is then left to warm up to room temperature and stirred at this temperature for 3 hours. 2000 Ml. of petroleum ether are then added, the mixture is left to stir 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-chloropyrimidine-3-oxide. Recrystallization yields analytically-pure product having a melting point of 193° C.

1. temperatureThe mixture is then cooled to 6°-8° C. and, at this temperature, there
2. additionare added dropwise within the course of 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. waitThe mixture is then left
6. temperatureto warm up to room temperature
7. stirringstirred at this temperature for 3 hours
8. waitthe mixture is left
9. stirringto stir for 1 hour
10. waitleft
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 record

ord-d34113bcc99e43e198cce663f85dd86d

Source dataset

uspto-grants-1980_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04220772