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
以SO24-/MxOy型固体超强酸为催化剂,采用固定床技术合成了N-甲基苯基吡咯烷酮。分别考察了原料物质的量的比、反应温度、进料速度3个因素对产品收率的影响。结果表明,最佳实验方案为:1,4-丁内酯与4-甲基苯胺的物质的量的比为1.4∶1、反...以SO24-/MxOy型固体超强酸为催化剂,采用固定床技术合成了N-甲基苯基吡咯烷酮。分别考察了原料物质的量的比、反应温度、进料速度3个因素对产品收率的影响。结果表明,最佳实验方案为:1,4-丁内酯与4-甲基苯胺的物质的量的比为1.4∶1、反应温度为320℃、进料速度为1.0 m L/min,此时1-(4-甲基苯基)-2-吡咯烷酮摩尔收率可以达到98.5%;1,4-丁内酯与2-甲基苯胺的物质的量之比为1.1∶1、反应温度为300℃、进料速度为1.0 m L/min时,1-(2-甲基苯基)-2-吡咯烷酮摩尔收率可达到91.1%。展开更多
2-hydroxy N methyl N phenyl acetamide was synthesized by using N methylaniline, chloracetyl chloride, anhydrous sodium acetate and methanol through the acetylation, esterfication and ester interchange steps. The acety...2-hydroxy N methyl N phenyl acetamide was synthesized by using N methylaniline, chloracetyl chloride, anhydrous sodium acetate and methanol through the acetylation, esterfication and ester interchange steps. The acetylation of N methylaniline with chloracetyl chloride, catalyzed by triethylamide with mole ratio n (C 6H 5NHCH 3)∶ n (ClCH 2C(O)Cl)∶ n (N(C 2H 5) 3)=1∶1.05∶1, the yield of 2 chloro N methyl N phenyl acetamide(Ⅰ) was 93.8%; Then the esterification of Ⅰ with anhydrous sodium acetate in the presence of phase transfer catalyst tetrabutyl ammonia bromide gave 97.3% yield of 2 acetoxyl N methyl N phenyl acetamide (Ⅱ); The ester interchange of with methanol catalyzed by potassium hydroxide gave 2 hydroxy N methyl N phenyl acetamide (Ⅲ) in 96.4% yield. And the total yield was 88.0%. IR and MS spectroscopy of products were analyzed and their characteristic peaks were assigned. Combining the results of elemental analysis, the molecular structure of Ⅰ, Ⅱ and Ⅲ was identified.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.
文摘以SO24-/MxOy型固体超强酸为催化剂,采用固定床技术合成了N-甲基苯基吡咯烷酮。分别考察了原料物质的量的比、反应温度、进料速度3个因素对产品收率的影响。结果表明,最佳实验方案为:1,4-丁内酯与4-甲基苯胺的物质的量的比为1.4∶1、反应温度为320℃、进料速度为1.0 m L/min,此时1-(4-甲基苯基)-2-吡咯烷酮摩尔收率可以达到98.5%;1,4-丁内酯与2-甲基苯胺的物质的量之比为1.1∶1、反应温度为300℃、进料速度为1.0 m L/min时,1-(2-甲基苯基)-2-吡咯烷酮摩尔收率可达到91.1%。
文摘2-hydroxy N methyl N phenyl acetamide was synthesized by using N methylaniline, chloracetyl chloride, anhydrous sodium acetate and methanol through the acetylation, esterfication and ester interchange steps. The acetylation of N methylaniline with chloracetyl chloride, catalyzed by triethylamide with mole ratio n (C 6H 5NHCH 3)∶ n (ClCH 2C(O)Cl)∶ n (N(C 2H 5) 3)=1∶1.05∶1, the yield of 2 chloro N methyl N phenyl acetamide(Ⅰ) was 93.8%; Then the esterification of Ⅰ with anhydrous sodium acetate in the presence of phase transfer catalyst tetrabutyl ammonia bromide gave 97.3% yield of 2 acetoxyl N methyl N phenyl acetamide (Ⅱ); The ester interchange of with methanol catalyzed by potassium hydroxide gave 2 hydroxy N methyl N phenyl acetamide (Ⅲ) in 96.4% yield. And the total yield was 88.0%. IR and MS spectroscopy of products were analyzed and their characteristic peaks were assigned. Combining the results of elemental analysis, the molecular structure of Ⅰ, Ⅱ and Ⅲ was identified.
