2,4,5-Triamino-6-hydroxypyrimidine sulfate synthesis

Yield:35011-47-3 98%

Reaction Conditions:

with 5%-palladium/activated carbon;sodium hydroxide in water at 60; under 7500.75 Torr; for 5 h;Inert atmosphere;Autoclave;

Steps:

26 Embodiment 26

Taking the 2, 4 - diamino -5 - nitroso -6 - hydroxy pyrimidine (3.14 g, 0 . 02 and 0.2 mol/L [...] solution 60 ml), 10 ml water is added to the high-pressure in the reactor, adding 5% of the metal catalyst is Pd/C, the high-pressure seal reactor, replace the nitrogen air 3 times, replace the nitrogen 3 times, inject the nitrogen to I MPa, heating to 60 °C, speed regulation to 500 r/min, reaction 5 hours, stop embraces mixes, cooling, air-bleed, operates the cauldron. Filtering, the filter cake melts may repeat use Pd, the filtrate is cooled to the room temperature, for 50% of the sulfuric acid accent to pH 2 - 3, the refrigerator rests over night, to separate out the yellow precipitate, filtered, cake 10 ml cold water washing, drying, get the yellow powder 2, 4, 5 - c amino -6 - hydroxy pyrimidine sulfate. Quality 4.58 g, 98%

References:

CN109535083,2019,A Location in patent:Paragraph 0088-0097