- Preparation method of caprolactam
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The invention provides a preparation method of caprolactam. According to the method, lysine or alpha-amino-epsilon-caprolactam and a salt thereof and alpha-(N,N-dimethylamino)-epsilon-caprolactam anda salt thereof are used as reaction raw materials, a transition metal supported by an acidic carrier is taken as a catalyst, methanol is taken as a solvent, and one-step catalytic conversion is carried out under the conditions that the temperature is 150-300 DEG C and the hydrogen pressure is 1-12 MPa, so that the process for producing caprolactam from lysine derived from biomass and other raw materials is realized. According to the invention, the reaction process is simple, the raw materials such as lysine, alpha-amino-epsilon-caprolactam and a salt thereof and alpha-(N, N-dimethylamino)-epsilon-caprolactam and a salt thereof can be derived from biomass, and have the advantages of being environmentally friendly, renewable and the like, the supported catalyst is easy to separate, and the transition metal catalyst supported by the acidic carrier is not easy to lose in the reaction process.
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Paragraph 0043-0045
(2020/06/20)
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- Seven-membered cyclic lysine derivative monomer and preparation method thereof, and antibacterial poly(epsilon-lysine) derivative and preparation method thereof
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The invention relates to a seven-membered cyclic lysine derivative monomer and a preparation method thereof, and an antibacterial poly(epsilon-lysine) derivative and a preparation method thereof. According to the invention, a lactam monomer is formed thro
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Paragraph 0063-0070
(2020/05/30)
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- One-pot conversion of lysine to caprolactam over Ir/H-Beta catalysts
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Amino acid lysine could serve as an ideal bio-based feedstock for the synthesis of caprolactam (CPL), which is currently a petroleum-derived monomer. Herein, we report the one-pot conversion of l-lysine to CPL via hydrogenolysis over bifunctional metal supported catalysts. Among the various hydrogenation metals and different supports, the combination of Ir and HB zeolite gave the best performance. Under optimal conditions, a 30% yield of CPL from l-lysine and a 58% yield from the reaction intermediate α-dimethyl amino caprolactam (DMAC) were obtained over a 2Ir/HB-124 catalyst at 250 °C in an autoclave or fixed-bed reactor. The reaction solvent dramatically affected the reaction selectivity, and methanol was found to be the best due to its unique contribution towards the formation of α-dimethyl amino caprolactam (DMAC) as well as the following C-N breakage of the C-N(CH3)2 bond. The acid sites on the catalyst accelerate lactam formation, and the synergy between the acid sites and hydrogenation sites favours C-N bond hydrogenolysis to produce CPL. Besides the acidity, the large pore size of HB is able to accommodate big reaction intermediate molecules inside the pores further ensures the superior performance of Ir/HB. The reaction route was identified, i.e., l-lysine first undergoes cyclization and N-methylation to DMAC, and then C-N(CH3)2 bond hydrogenolysis to form CPL. The Ir/HB catalyst has reasonably good stability and high selectivity, making this one-pot conversion process a novel and environmentally benign way of producing CPL from easily available renewable feedstocks.
- Sebastian, Joby,Zheng, Mingyuan,Jiang, Yu,Zhao, Yu,Wang, Hua,Song, Zhendong,Li, Xinsheng,Pang, Jifeng,Zhang, Tao
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supporting information
p. 2462 - 2468
(2019/05/21)
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- Preparation, characterization, DNA binding, and in Vitro cytotoxicity of the enantiomers of the platinum(II) complexes N-methyl-, N-ethyl- and N,N- dimethyl-(R)- and -(S)-3-aminohexahydroazepinedichloroplatinum(II)
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A series of chiral diaminedichloroplatinum(II) complexes derived from [Pt(ahaz)Cl2] (ahaz = 3-aminohexahydroazepine) have been synthesized and tested for cytotoxic activity. Novel synthetic pathways were developed to produce the structural derivatives of the ahaz ligand, with alkyl substituents on the exocyclic nitrogen atom. The platinum(II) complexes of these ligands were synthesized and characterized by NMR and CD spectroscopy, confirming isomeric and enantiomeric purity. The crystal structures of three of these complexes, [Pt(S-meahaz)Cl2], [Pt(R-etahaz)Cl2], and [Pt(S- dimeahaz)Cl2] (meahaz = N-methylahaz, etahaz = N-ethylahaz, dimeahaz = N,N- dimethylahaz), have been determined to establish the orientation of the protons and alkyl substituents on the nitrogen donor atoms. In vitro assays of the cytotoxic activity of the complexes have revealed a significant and reproducible enantioselective trend with the R-enantiomers more active than the S-enantiomers in all cell lines. Increasing the steric bulk on the amine groups was found to have only a modest effect on activity. No enantioselectivity was observed in the binding of R- and S-[Pt(etahaz)Cl2] to calf-thymus DNA.
- Rezler, Evonne M.,Fenton, Ronald R.,Esdale, Warren J.,McKeage, Mark J.,Russell, Pamela J.,Hambley, Trevor W.
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p. 3508 - 3515
(2007/10/03)
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