Method for preparation of 5-methyl-2-pyrazinemethanol from dihydroxyacetone
A technology of dihydroxyacetone and pyrazine methanol, which is applied in the direction of organic chemistry, can solve the problems of operators' health and environmental safety hazards, expensive reaction raw materials, and long reaction routes, etc., and achieves easy industrial production, high selectivity, and steps simple effect
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Embodiment 1
[0013] Dissolve 0.1355g of dihydroxyacetone (DHA) and 0.1986g of diammonium hydrogen phosphate in 15ml of water, then add them into a closed reactor and heat up to a reaction temperature of 100°C for reaction. After 60 minutes of reaction, the reactor is lowered to room temperature. The liquid reaction products were taken out, qualitatively analyzed by gas chromatography-mass spectrometry, and quantitatively analyzed by liquid chromatography and gas chromatography.
Embodiment 2
[0015] 5-Methyl-2-pyrazinemethanol (MPM) was synthesized under different pH conditions. Dihydroxyacetone reacts with diammonium hydrogen phosphate and reacts under different pH values, except adding 85% phosphoric acid and 25% ammoniacal liquor of different consumptions in the reaction as pH adjuster, reaction condition is the same as embodiment 1, reaction pH and target product The yields are listed in Table (1).
[0016] Table 1. Reaction of dihydroxyacetone and diammonium hydrogen phosphate under different pH conditions to generate 5-methyl-2-pyrazine methanol conversion selectivity yield situation
[0017]
[0018] As can be seen from the table, different pHs have an impact on the yield of the target product, and wherein the 5-methyl-2-pyrazinemethanol with a better yield is obtained when the pH is in the vicinity of 8-9.
Embodiment 3
[0020] Synthesis of 5-methyl-2-pyrazinemethanol (MPM) at different reaction temperatures. Except adding 100 μl of ammonia water as a pH regulator and different reaction temperatures, the reaction conditions were the same as in Example 1, and the reaction temperature and the yield of the target product were listed in Table (two).
[0021] Table two, the reaction of dihydroxyacetone and diammonium hydrogen phosphate to generate 5-methyl-2-pyrazine methanol conversion selectivity yield under different temperatures
[0022]
[0023] As can be seen from the table, at different reaction temperatures, dihydroxyacetone and ammonium salts can react effectively, and the preferred reaction temperature is 90-110°C to obtain 5-methyl-2-pyrazinemethanol with a better yield .
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