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With selenium(IV) oxide; sodium acetate; In water;
1. 2,4-DIAMINO-6-HYDROXYMETHYLPTERIDINE SPC2 A solution of 6.4 grams of barium chloride in a minimum amount of hot water was added with stirring at a temperature of 70-80 C to a suspension of 7.6 grams of 2,4,5,6-tetraaminopyrimidine sulphate in 104 ml water. The resulting suspension was stirred for 30 minutes and the formed barium sulphate was removed by filtration and washed on the funnel with 26 ml water at a temperature of 70 C. The solution containing the 2,4,5,6-tetraaminopyrimidine dihydrochloride is diluted with water to a final volume of 400 ml. A solution of 128 grams of sodium acetate, 136 grams of bisulphite addition product of 1,3-dihydroxyacetone (free of methyl glyoxal) and 46 grams of cysteine hydrochloride in 390 ml water was prepared at room temperature in a 2 liter three-necked flask fitted with a stirrer, an air-bubbling system and a dropping funnel. To this solution, the 400 ml of the previously prepared solution of 2,4,5,6-tetraaminopyrimidine dihydrochloride were added with energic stirring and air-bubbling. A solution of 8 g of selenium dioxide dissolved in the minimum amount of water was made. Half of this solution was added to the reaction mixture immediately after the addition of the tetraaminopyrimidine solution and the other half 4-7 hours later. The reaction was allowed to proceed for 24 hours at room temperature. The reaction can be carried out in a similar manner in a range of temperatures from 20 to 100 C, but the yield is lower. After the end of the reaction, the solution is kept 1 hour at 4 C. The precipitate was filtered off, washed on the funnel with cold alcohol, alcohol:ethyl ether (1:1) and ethyl ether, then dried under vacuum for 24 hours at 50. The yield is 3,8 g (72 %) of 2,4-diamino-6-hydroxymethylpteridine.
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