1,2-diiodo-3,3-dimethylbut-1-ene was synthesized used 3,3-dimethylbut-1-yne as the initial materials and Ce2(SO4)3 as catalyst in H2O.Then 5,5-dimethyl-1-(o-aminophenyl)-1,3-hexadiyne was synthesized from 1,2-diiodo-3...1,2-diiodo-3,3-dimethylbut-1-ene was synthesized used 3,3-dimethylbut-1-yne as the initial materials and Ce2(SO4)3 as catalyst in H2O.Then 5,5-dimethyl-1-(o-aminophenyl)-1,3-hexadiyne was synthesized from 1,2-diiodo-3,3-dimethylbut-1-ene and 2-ethynylaniline by cross-coupling rection in the presence of Pd(OAc)2 and CuI.The total yield was 68.7 %.The structure was characterized by NMR and MS spectrum.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1,2-diiodo-3,3-dimethylbut-1-ene was synthesized used 3,3-dimethylbut-1-yne as the initial materials and Ce2(SO4)3 as catalyst in H2O.Then 5,5-dimethyl-1-(o-aminophenyl)-1,3-hexadiyne was synthesized from 1,2-diiodo-3,3-dimethylbut-1-ene and 2-ethynylaniline by cross-coupling rection in the presence of Pd(OAc)2 and CuI.The total yield was 68.7 %.The structure was characterized by NMR and MS spectrum.
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。
