Реакция #75108

Уравнение реакции

2,4-diamino-6-chloropyrimidine

ethanol

peracetic acid

→

2,4-diamino-6-chloropyrimidine-3-oxide

Растворители

acetic

—

petroleum ether

Условия реакции

Обработка

1. 1
   ТемператураThe mixture is then cooled to 6°-8° C. and, at this temperature, there
2. 2
   workup.ADDITIONare added dropwise within the course of 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.WAITThe mixture is then left
6. 6
   Температураto warm up to room temperature
7. 7
   workup.STIRRINGstirred at this temperature for 3 hours
8. 8
   workup.WAITthe mixture is left
9. 9
   workup.STIRRINGto stir for 1 hour
10. 10
    workup.WAITleft
11. 11
    ФильтрацияThe separated precipitate is filtered off
12. 12
    Промывкаback-washed with 200 ml
13. 13
    Сушкаof petroleum ether and dried under reduced pressure, there

Методика

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. 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.

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