Reaction of the β diketimine compound (2,6 Me 2C 6H 3)NC(Me)CHC(Me)N(C 6H 3 2,6 Me 2)H (LH,1) with 1 equiv of n BuLi/hexane in THF,followed by crystallization from toluene,affords the β diketiminate lithium complex ...Reaction of the β diketimine compound (2,6 Me 2C 6H 3)NC(Me)CHC(Me)N(C 6H 3 2,6 Me 2)H (LH,1) with 1 equiv of n BuLi/hexane in THF,followed by crystallization from toluene,affords the β diketiminate lithium complex LLi(THF)(2)in high yields.The crystal structure of complex 2 was determined by X ray diffraction method.It crystallizes in monoclinic,space group P 2/(1)/ n with a =1 4036(5), b =1 3261(4), c =1 4248(5)nm, β =115 437(6)°, V =2 3950(13)nm 3,and D c =1 066Mg·m -3 for Z =4.In the structure,the metallacycle is almost fully planar,and the Li atom is coordinated by two nitrogen atoms of the β diketiminate ligand and one oxygen atom of THF molecule.展开更多
采用单因素法,以2-氯-4,6-二(N-丁基-2,2,6,6-四甲基-4-哌啶胺基)-1,3,5-三嗪、环己烷、叔丁基过氧化氢为原料,三氧化钼为催化剂合成2-氯-4,6-二(N-丁基-1-环己氧基-2,2,6,6-四甲基-4-哌啶胺基)-1,3,5-三嗪。结果表明,最佳工艺条件为反...采用单因素法,以2-氯-4,6-二(N-丁基-2,2,6,6-四甲基-4-哌啶胺基)-1,3,5-三嗪、环己烷、叔丁基过氧化氢为原料,三氧化钼为催化剂合成2-氯-4,6-二(N-丁基-1-环己氧基-2,2,6,6-四甲基-4-哌啶胺基)-1,3,5-三嗪。结果表明,最佳工艺条件为反应温度95℃,反应时间14 h,原料物质的量比n(2-氯-4,6-二(N-丁基-2,2,6,6-四甲基-4-哌啶胺基)-1,3,5-三嗪)∶n(环己烷)∶n(叔丁基过氧化氢)为0.01∶0.45∶0.2,催化剂三氧化钼用量为0.4 g (相对0.01 mol2-氯-4,6-二(N-丁基-2,2,6,6-四甲基-4-哌啶胺基)-1,3,5-三嗪),产品收率为93.50%。展开更多
A compound ethyl(5S,6R)-2-(4-methylphenyl)-6-[(1R)-tert-butyldimethylsilyloxyethy]-penem-3-carboxylate was synthesized through displacement,acylation and Wittig cyclization reaction of optically active material(3R,4R)...A compound ethyl(5S,6R)-2-(4-methylphenyl)-6-[(1R)-tert-butyldimethylsilyloxyethy]-penem-3-carboxylate was synthesized through displacement,acylation and Wittig cyclization reaction of optically active material(3R,4R)-3-[(1R)-tert-butyldimethylsilyloxyethyl]-4-acetoxy-2-azetidi-none(4AA)upon thionocarboxlic acid.The intermediates and the target product were characterized by 1HNMR,IR,elementary analysis and MS.展开更多
文摘Reaction of the β diketimine compound (2,6 Me 2C 6H 3)NC(Me)CHC(Me)N(C 6H 3 2,6 Me 2)H (LH,1) with 1 equiv of n BuLi/hexane in THF,followed by crystallization from toluene,affords the β diketiminate lithium complex LLi(THF)(2)in high yields.The crystal structure of complex 2 was determined by X ray diffraction method.It crystallizes in monoclinic,space group P 2/(1)/ n with a =1 4036(5), b =1 3261(4), c =1 4248(5)nm, β =115 437(6)°, V =2 3950(13)nm 3,and D c =1 066Mg·m -3 for Z =4.In the structure,the metallacycle is almost fully planar,and the Li atom is coordinated by two nitrogen atoms of the β diketiminate ligand and one oxygen atom of THF molecule.
文摘采用单因素法,以2-氯-4,6-二(N-丁基-2,2,6,6-四甲基-4-哌啶胺基)-1,3,5-三嗪、环己烷、叔丁基过氧化氢为原料,三氧化钼为催化剂合成2-氯-4,6-二(N-丁基-1-环己氧基-2,2,6,6-四甲基-4-哌啶胺基)-1,3,5-三嗪。结果表明,最佳工艺条件为反应温度95℃,反应时间14 h,原料物质的量比n(2-氯-4,6-二(N-丁基-2,2,6,6-四甲基-4-哌啶胺基)-1,3,5-三嗪)∶n(环己烷)∶n(叔丁基过氧化氢)为0.01∶0.45∶0.2,催化剂三氧化钼用量为0.4 g (相对0.01 mol2-氯-4,6-二(N-丁基-2,2,6,6-四甲基-4-哌啶胺基)-1,3,5-三嗪),产品收率为93.50%。
文摘A compound ethyl(5S,6R)-2-(4-methylphenyl)-6-[(1R)-tert-butyldimethylsilyloxyethy]-penem-3-carboxylate was synthesized through displacement,acylation and Wittig cyclization reaction of optically active material(3R,4R)-3-[(1R)-tert-butyldimethylsilyloxyethyl]-4-acetoxy-2-azetidi-none(4AA)upon thionocarboxlic acid.The intermediates and the target product were characterized by 1HNMR,IR,elementary analysis and MS.
