对以邻硝基甲苯为主要原料,经锌粉 氯化铵溶液还原、氯甲酸甲酯酰基化、硫酸二甲酯甲基化合成N 甲氧基 N 2 甲基苯基氨基甲酸甲酯的工艺路线进行了研究.重点考察了还原反应中溶剂种类、还原温度对反应的影响以及N 羟基 N 2 甲苯氨基甲...对以邻硝基甲苯为主要原料,经锌粉 氯化铵溶液还原、氯甲酸甲酯酰基化、硫酸二甲酯甲基化合成N 甲氧基 N 2 甲基苯基氨基甲酸甲酯的工艺路线进行了研究.重点考察了还原反应中溶剂种类、还原温度对反应的影响以及N 羟基 N 2 甲苯氨基甲酸甲酯的纯化方法.N 羟基 N 2 甲苯基氨基甲酸甲酯、N 甲氧基 N 2 甲苯基氨基甲酸甲酯均经MS,1HNMR确认.展开更多
A convenient and highly efficient method is described for the synthesis of N-methoxycarbazole derivatives,including those with sterically demanding,benzannulated,or strongly electron-donating or-withdrawing substituen...A convenient and highly efficient method is described for the synthesis of N-methoxycarbazole derivatives,including those with sterically demanding,benzannulated,or strongly electron-donating or-withdrawing substituents.Various N-methoxycarbazole derivatives were directly prepared in good-to-moderate yields by the Pd_(2)(dba)_(3)CHCl_(3)/9,9-dimethyl-4,5-bis(diphenylphosphino)xanthene-catalyzed reactions of the corresponding dibromobiphenyl compounds and methoxyamine.Based on this methodology,the first total synthesis of 3,3′-[oxybis(methylene)]bis(9-methoxy-9H-carbazole),an antimicrobial dimeric carbazole alkaloid previously isolated from the stem bark of Murraya koenigii,was achieved in 18% yield over seven steps from 1,2-dibromobenzene.展开更多
文摘对以邻硝基甲苯为主要原料,经锌粉 氯化铵溶液还原、氯甲酸甲酯酰基化、硫酸二甲酯甲基化合成N 甲氧基 N 2 甲基苯基氨基甲酸甲酯的工艺路线进行了研究.重点考察了还原反应中溶剂种类、还原温度对反应的影响以及N 羟基 N 2 甲苯氨基甲酸甲酯的纯化方法.N 羟基 N 2 甲苯基氨基甲酸甲酯、N 甲氧基 N 2 甲苯基氨基甲酸甲酯均经MS,1HNMR确认.
基金supported by the Natural Science Foundation of Tianjin,China(No.15JCYBJC20100).
文摘A convenient and highly efficient method is described for the synthesis of N-methoxycarbazole derivatives,including those with sterically demanding,benzannulated,or strongly electron-donating or-withdrawing substituents.Various N-methoxycarbazole derivatives were directly prepared in good-to-moderate yields by the Pd_(2)(dba)_(3)CHCl_(3)/9,9-dimethyl-4,5-bis(diphenylphosphino)xanthene-catalyzed reactions of the corresponding dibromobiphenyl compounds and methoxyamine.Based on this methodology,the first total synthesis of 3,3′-[oxybis(methylene)]bis(9-methoxy-9H-carbazole),an antimicrobial dimeric carbazole alkaloid previously isolated from the stem bark of Murraya koenigii,was achieved in 18% yield over seven steps from 1,2-dibromobenzene.
