Reaktion #1722948

Reaktionsgleichung

sodium hydroxide

2-amino-4-hexylamino-6-chloropyrimidine

phthalic anhydride

sodium hydrogen sulfite

→

expected compound

Ausbeute 42.2%

2-amino-4-hexylamino-6-chloropyrimidine 3-oxide

Ausbeute 42.2%

Lösungsmittel

isopropyl ether

water

isopropanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeat +30° C
2. 2
   SonstigeAfter reaction for 3 hours
3. 3
   Sonstigeto destroy the
4. 4
   Sonstigeto separate out
5. 5
   Einengenthe upper phase was concentrated under vacuum
6. 6
   SonstigeThe residue obtained
7. 7
   SonstigeThe solid obtained
8. 8
   FiltrationThe solid was filtered off
9. 9
   Waschenwashed
10. 10
    SonstigeIt was dried in a heated desiccator

Vorschrift

5.95 g of urea/H2O2 complex and 9.07 g of phthalic anhydride were suspended in 90 ml of isopropanol, in a three-necked flask. The mixture was stirred for 30 min at room temperature (20-25° C.). 10 g of 2-amino-4-hexylamino-6-chloropyrimidine were then added while controlling the exotherm at +30° C. After reaction for 3 hours, 100 ml of sodium hydrogen sulfite were poured thereinin to destroy the residual oxidizing agents. The mixture was permitted to separate out by settling and the upper phase was concentrated under vacuum. The residue obtained was taken up in a water (80 ml)/30% sodium hydroxide (20 ml) mixture. The solid obtained was reimpasted in 150 ml of isopropyl ether. The solid was filtered off and washed. It was dried in a heated desiccator. 4.52 g of the expected compound were thus obtained, for a yield of 42%.

Quelle