A six-arm initiating core containing 1,3,5-triazine:N,N’,N″-tris-(4,6-dichloro——triazine-2-yl)-diethylenetriamine(3T-DETA)is synthesize from cyanuric chloride(TCT)and diethylenetriamine(DETA).The optimum reaction ...A six-arm initiating core containing 1,3,5-triazine:N,N’,N″-tris-(4,6-dichloro——triazine-2-yl)-diethylenetriamine(3T-DETA)is synthesize from cyanuric chloride(TCT)and diethylenetriamine(DETA).The optimum reaction conditions include that n(TCT)∶n(DETA)=4∶1,N,N-diisopropylethylamine(DIPEA)is used as base,n(DIPEA)∶n(DETA)=4∶1,tetrahydrofuran as solvent,the flow rate of the THF solution of DETA and DIPEA is 0.67 mL/min,reacted at 0-5℃for 4 h and then at room temperature for 48 h,the product yield could reach to 95.3%.The structure of the target product is characterized by elementary analysis,MS,1H-NMR and FTIR.展开更多
A 1,3,5-triazin derivative: N,N’-bis-(4,6-dichloro——triazin-2-yl)-hexane-1,6-diamine was prepared from cyanuric chloride and hexane-1,6-diamine by nucleophilic substitution reaction.By trying experiments,the molar ...A 1,3,5-triazin derivative: N,N’-bis-(4,6-dichloro——triazin-2-yl)-hexane-1,6-diamine was prepared from cyanuric chloride and hexane-1,6-diamine by nucleophilic substitution reaction.By trying experiments,the molar ratio of cyanuric chloride to hexane-1,6-diamine was 2:1,using sodium hydroxide as base and the mixture of dichlormethane and water as solvent.On the basis of these results,a L9(33) orthogonal layout was designed to investigate the effects of the reaction time,the variety and dosage of base as well as the vomule ratio of dichlormethane and water on the yields of products.Three levels were selected for every factor.The result showed that when the molar ratio of sodium hydroxide to hexane-1,6-diamine was 2:1,the volume ratio of dichloromethane and water was 1:1 and the reaction was carried out at 0-5 ℃ for 6 h,the product yield could reach to 92.8%.The structure of the target product was characterized by elementary analysis,MS,1 H-NMR and FTIR.展开更多
文摘A six-arm initiating core containing 1,3,5-triazine:N,N’,N″-tris-(4,6-dichloro——triazine-2-yl)-diethylenetriamine(3T-DETA)is synthesize from cyanuric chloride(TCT)and diethylenetriamine(DETA).The optimum reaction conditions include that n(TCT)∶n(DETA)=4∶1,N,N-diisopropylethylamine(DIPEA)is used as base,n(DIPEA)∶n(DETA)=4∶1,tetrahydrofuran as solvent,the flow rate of the THF solution of DETA and DIPEA is 0.67 mL/min,reacted at 0-5℃for 4 h and then at room temperature for 48 h,the product yield could reach to 95.3%.The structure of the target product is characterized by elementary analysis,MS,1H-NMR and FTIR.
文摘A 1,3,5-triazin derivative: N,N’-bis-(4,6-dichloro——triazin-2-yl)-hexane-1,6-diamine was prepared from cyanuric chloride and hexane-1,6-diamine by nucleophilic substitution reaction.By trying experiments,the molar ratio of cyanuric chloride to hexane-1,6-diamine was 2:1,using sodium hydroxide as base and the mixture of dichlormethane and water as solvent.On the basis of these results,a L9(33) orthogonal layout was designed to investigate the effects of the reaction time,the variety and dosage of base as well as the vomule ratio of dichlormethane and water on the yields of products.Three levels were selected for every factor.The result showed that when the molar ratio of sodium hydroxide to hexane-1,6-diamine was 2:1,the volume ratio of dichloromethane and water was 1:1 and the reaction was carried out at 0-5 ℃ for 6 h,the product yield could reach to 92.8%.The structure of the target product was characterized by elementary analysis,MS,1 H-NMR and FTIR.
