Reaktion #432608

Reaktionsgleichung

HNO3

material

4,6-Dihydroxy-2-methoxypyrimidine

→

title compound

Ausbeute 68.0%

4,6-Dihydroxy-2-methoxy-5-nitropyrimidine

Ausbeute 68.0%

Lösungsmittel

HOAc

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwith cooling
2. 2
   Sonstigewas kept below 20° C
3. 3
   TemperaturThis stirred mixture was cooled in an ice bath
4. 4
   Temperaturwas maintained between 18°-20° C
5. 5
   workup.STIRRINGThe reaction was then stirred overnight
6. 6
   SonstigeThe precipitate which formed
7. 7
   Filtrationwas filtered off
8. 8
   Waschenwashed with HOAc (50 mL)
9. 9
   Filtrationfiltered off
10. 10
    Sonstigedried to constant weight in vacuo at 60° C.

Vorschrift

To glacial HOAc (860 mL) was added red fuming HNO3 (300 mL) with cooling and stirring, at such a rate that the temperature was kept below 20° C. This stirred mixture was cooled in an ice bath and the foregoing material prepared in Example 134 (200 g, 78% pure, 1.1 mol) was added in portions over a period of 1 hr such that the temperature was maintained between 18°-20° C. The reaction was then stirred overnight. The precipitate which formed was filtered off and washed with HOAc (50 mL). This solid was then slurried with ice-H2O (400 mL), filtered off and dried to constant weight in vacuo at 60° C. to yield 141 g (0.75 mol, 68% yield) of the title compound; nmr (d6 -DMSO) d: 3.95 (s); mass spectrum showed m/e 187 (M+). A separate synthesis gave an analytical sample.

Quelle