The hydrochloride of 1-(1-amino-3-methyl)butyl borate pinacol is prepared by using the isobutylbromide to form the Grignard agent.The product is protected with the pinacol,then reacted with the lithium diisopropylamid...The hydrochloride of 1-(1-amino-3-methyl)butyl borate pinacol is prepared by using the isobutylbromide to form the Grignard agent.The product is protected with the pinacol,then reacted with the lithium diisopropylamide and the anhydrous zinc chloride.Finally,the product is synthesized in the existence of the LHMDS.All the compounds are confirmed by MS and 1H-NMR.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The hydrochloride of 1-(1-amino-3-methyl)butyl borate pinacol is prepared by using the isobutylbromide to form the Grignard agent.The product is protected with the pinacol,then reacted with the lithium diisopropylamide and the anhydrous zinc chloride.Finally,the product is synthesized in the existence of the LHMDS.All the compounds are confirmed by MS and 1H-NMR.
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。
