以甲酸和氢氧化钾为原料,不外加任何溶剂一步合成二甲酸钾。通过单因素实验,考察了原料配比、反应温度和反应时间对产品质量与收率的影响。采用正交实验进一步优化了合成工艺,确定了最佳工艺条件:n(HCOOH)/n(KOH)=2.2、反应温度70℃、...以甲酸和氢氧化钾为原料,不外加任何溶剂一步合成二甲酸钾。通过单因素实验,考察了原料配比、反应温度和反应时间对产品质量与收率的影响。采用正交实验进一步优化了合成工艺,确定了最佳工艺条件:n(HCOOH)/n(KOH)=2.2、反应温度70℃、反应时间30 m in,在该条件下,二甲酸钾产品收率达98%以上。所得产品经红外光谱分析及熔点测定,其结果与文献报道一致。反应过程绿色化,有很好的原子经济性。展开更多
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
文摘以甲酸和氢氧化钾为原料,不外加任何溶剂一步合成二甲酸钾。通过单因素实验,考察了原料配比、反应温度和反应时间对产品质量与收率的影响。采用正交实验进一步优化了合成工艺,确定了最佳工艺条件:n(HCOOH)/n(KOH)=2.2、反应温度70℃、反应时间30 m in,在该条件下,二甲酸钾产品收率达98%以上。所得产品经红外光谱分析及熔点测定,其结果与文献报道一致。反应过程绿色化,有很好的原子经济性。
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.
