反应详情

Sodium dithionite was added portionwise to a warm solution of 2-amino-4-hydroxy-6-(1,1-diethyl-3-hydroxy-2-hydroxyiminopropylamino)-5-nitropyrimidine (450 mg) in 0.1M sodium hydroxide until the colour changed from red to very pale yellow. A solid product was not obtained either on cooling or on adjusting the pH. In order to separate the product from inorganic material the solution was evaporated and the product extracted with ethanol and the inorganic material was filtered off. This extraction was repeated and the combined extracts were evaporated to dryness in vacuo. The residue was dissolved in the minimum quantity of water and placed on a column of Amberlite (C.G.50) ion exchange resin (2.5×28 cm.). Elution with water gave two main fluorescent bands. Evaporation of solution containing the first band gave the 6-carboxaldehyde derivative of the title compound (10 mg., 3%) as a bright orange powder. The second band gave the 7,8-dihydropteridine (160 mg., 44.5%) as a yellow powder.

1. customA solid product was not obtained
2. temperatureon cooling
3. customIn order to separate the product from inorganic material the solution
4. customwas evaporated
5. extractionthe product extracted with ethanol
6. filtrationthe inorganic material was filtered off
7. extractionThis extraction
8. customthe combined extracts were evaporated to dryness in vacuo
9. dissolutionThe residue was dissolved in the minimum quantity of water
10. washElution with water
11. customgave two main fluorescent bands
12. customEvaporation of solution
13. additioncontaining the first band