Methyl-2-butene reacted with isoamyl nitrite in concentrated hydrochloric acid to obtain 2-chloro-2-methyl-3-nitrosobutane which was condensed with 1,4-butanediamine to give 3, 3, 10, 10-tetramethyl-4, 9-diazadodecan-...Methyl-2-butene reacted with isoamyl nitrite in concentrated hydrochloric acid to obtain 2-chloro-2-methyl-3-nitrosobutane which was condensed with 1,4-butanediamine to give 3, 3, 10, 10-tetramethyl-4, 9-diazadodecan-2, 11-dione dioxime (Prognox HL91) in an overall yield of 14.5%.展开更多
phenanthroline(1) was oxidized by a mixture of concentrated sulfuric acid and concentrated nitric acid in the presence of sodium bromide to yield 1,10 phenanthroline 5,6 dione(2) in 90%. Compound 2 gave a mono oxime(3...phenanthroline(1) was oxidized by a mixture of concentrated sulfuric acid and concentrated nitric acid in the presence of sodium bromide to yield 1,10 phenanthroline 5,6 dione(2) in 90%. Compound 2 gave a mono oxime(3) hydrochloric salt in nearly quantitive amount by reacting with equal molar hydroxylamine hydrochloride. The structures of the compounds were characterized by IR and 1 H NMR spectroscopy. The method is more simple and efficient.展开更多
Benzhydrylamine was synthesized from benzophenoneoxime formed by oximation of benzophenone inan overall yield of 83.5%. The reduction took place with Zn in 20% NaOH solution at 100℃ for 7h in a yield of 84.7% andpuri...Benzhydrylamine was synthesized from benzophenoneoxime formed by oximation of benzophenone inan overall yield of 83.5%. The reduction took place with Zn in 20% NaOH solution at 100℃ for 7h in a yield of 84.7% andpurity of 99.1%.展开更多
文摘Methyl-2-butene reacted with isoamyl nitrite in concentrated hydrochloric acid to obtain 2-chloro-2-methyl-3-nitrosobutane which was condensed with 1,4-butanediamine to give 3, 3, 10, 10-tetramethyl-4, 9-diazadodecan-2, 11-dione dioxime (Prognox HL91) in an overall yield of 14.5%.
文摘phenanthroline(1) was oxidized by a mixture of concentrated sulfuric acid and concentrated nitric acid in the presence of sodium bromide to yield 1,10 phenanthroline 5,6 dione(2) in 90%. Compound 2 gave a mono oxime(3) hydrochloric salt in nearly quantitive amount by reacting with equal molar hydroxylamine hydrochloride. The structures of the compounds were characterized by IR and 1 H NMR spectroscopy. The method is more simple and efficient.
文摘Benzhydrylamine was synthesized from benzophenoneoxime formed by oximation of benzophenone inan overall yield of 83.5%. The reduction took place with Zn in 20% NaOH solution at 100℃ for 7h in a yield of 84.7% andpurity of 99.1%.
