2-nitro-10-hydroxy-5,10-dihydrophenophosphazine-10-oxide can be reduced easily with hydrous hydrazine by Fe/MgO catalyst.The reduced compound was detected by IR and HNMR.It showed that the reduction yield is 94%.The c...2-nitro-10-hydroxy-5,10-dihydrophenophosphazine-10-oxide can be reduced easily with hydrous hydrazine by Fe/MgO catalyst.The reduced compound was detected by IR and HNMR.It showed that the reduction yield is 94%.The catalyst can be used in reduction for three times.This reduction method has a lower cost,less pollution to environment and suit to the industrializing demand for dye intermediate production.展开更多
以亚氨基二乙腈为起始原料,经过亚硝基化、环合、硝化三步反应得到2,6-二氨基-3,5-二硝基吡嗪-1-氧化物(LLM-105)。确定了硝化2,6-二氨基吡嗪-1-氧化物(DAPO)制备LLM-105的最佳工艺条件为:反应温度25℃,反应时间5h,用发烟硝酸或硝酸钾...以亚氨基二乙腈为起始原料,经过亚硝基化、环合、硝化三步反应得到2,6-二氨基-3,5-二硝基吡嗪-1-氧化物(LLM-105)。确定了硝化2,6-二氨基吡嗪-1-氧化物(DAPO)制备LLM-105的最佳工艺条件为:反应温度25℃,反应时间5h,用发烟硝酸或硝酸钾向发烟硫酸和2,6-二氨基吡嗪-1-氧化物混合物中加料的工艺路线,总产率为35%。用1 H NMR,IR,MS对DAPO和LLM-105的结构进行了表征,推测了DAPO环化反应历程。展开更多
文摘2-nitro-10-hydroxy-5,10-dihydrophenophosphazine-10-oxide can be reduced easily with hydrous hydrazine by Fe/MgO catalyst.The reduced compound was detected by IR and HNMR.It showed that the reduction yield is 94%.The catalyst can be used in reduction for three times.This reduction method has a lower cost,less pollution to environment and suit to the industrializing demand for dye intermediate production.
文摘以亚氨基二乙腈为起始原料,经过亚硝基化、环合、硝化三步反应得到2,6-二氨基-3,5-二硝基吡嗪-1-氧化物(LLM-105)。确定了硝化2,6-二氨基吡嗪-1-氧化物(DAPO)制备LLM-105的最佳工艺条件为:反应温度25℃,反应时间5h,用发烟硝酸或硝酸钾向发烟硫酸和2,6-二氨基吡嗪-1-氧化物混合物中加料的工艺路线,总产率为35%。用1 H NMR,IR,MS对DAPO和LLM-105的结构进行了表征,推测了DAPO环化反应历程。