Improvement of the Synthesis Process of 2,6-Diamino-3,5-Dinitropyrazine-1-Oxide
Fude Nie
Abstract
Fude Nie
Abstract
LLM-105 was prepared by methoxytation,nitration,amination,and oxidation using 2,6-dichloropyrazine as starting materials.The effects of methoxylation reaction condition,different nitration system,different amination system and volume ratio of trifluoroacetic acid and hydrogen peroxide on the total yield of LLM-105 were investigated.Optimized synthesis conditions are 25% sodium methoxide methanol solution,reflux for 3 h.2,6-Dimethoxypyrazine as intermediate for nitration,20%oleum and potassium nitrate nitration system,the reaction at room temperature for 3 h.Aprotic solvent ethanol as amide solvents,the reaction under the conditions of 60℃ for 2 h.The volume ratio of trifluoroacetic acid and 30% hydrogen peroxide as 3∶2,the reaction under the conditions of 45℃ for 6 h.The total yield of LLM-105 is 54%.
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LLM-105 was prepared by methoxytation,nitration,amination,and oxidation using 2,6-dichloropyrazine as starting materials.The effects of methoxylation reaction condition,different nitration system,different amination system and volume ratio of trifluoroacetic acid and hydrogen peroxide on the total yield of LLM-105 were investigated.Optimized synthesis conditions are 25% sodium methoxide methanol solution,reflux for 3 h.2,6-Dimethoxypyrazine as intermediate for nitration,20%oleum and potassium nitrate nitration system,the reaction at room temperature for 3 h.Aprotic solvent ethanol as amide solvents,the reaction under the conditions of 60℃ for 2 h.The volume ratio of trifluoroacetic acid and 30% hydrogen peroxide as 3∶2,the reaction under the conditions of 45℃ for 6 h.The total yield of LLM-105 is 54%.
Key concepts: Nitration, Chemistry, Trifluoroacetic acid, Sodium methoxide, Yield (engineering), Nitric acid, Methanol, Hydrogen peroxide