- A 2, 4 - dioxo -3 - aza spiro - [5, 5] undecane - 1, 5 - dinitrile preparation method (by machine translation)
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The present invention provides a 2, 4 - dioxo - 3 - aza-spiro - [5, 5] undecane - 1, 5 - dinitrile preparation method, comprises the following steps: ammonia methanol solution dropping to cyclohexanone and cyanoacetic acid methyl ester in the mixed solution of, thermal insulation reaction, a 2, 4 - dioxo - 3 - aza-spiro - [5, 5] undecane - 1, 5 - [...] solution; then adding water mix, dropping a sulfuric acid solution, thermal insulation reaction, separation, washing, shall be 2, 4 - dioxo - 3 - aza-spiro - [5, 5] undecane - 1, 5 - a dinitrile. The invention provides a 2, 4 - dioxo - 3 - aza-spiro - [5, 5] undecane - 1, 5 - dinitrile preparation method, the process is simple, low in energy consumption, less side reaction, the product yield can reach 98.5% or more, the product of the ammonia nitrogen in the content of less than 0.3%, cyanoacetate of methyl acetate and the unit consumption of 0.85 - 1.1 t/t, is suitable for large-scale industrial production. (by machine translation)
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Paragraph 0009; 0035; 0036; 0038; 0040; 0041; 0043; 0045
(2019/03/08)
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- Process for the preparation of gabapentin hydrochloride
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A process for preparation of gabapentin hydrochloride by converting 1,5-dicyano-2,4-dioxo-3-azaspiro[5,5]-undecane into 1,5-diaminoformyl-2,4-dioxo-3-azaspiro[5,5]-undecane at a temperature of 65° C. to 85° C. in the presence of a strong acid, and then carrying out Hofmann rearrangement under an alkaline condition. The starting material of the process is readily available. The process is simple, and can reduce the purification procedure of intermediates, reduce production cost, and obtain product with higher purity.
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Page/Page column 3-4
(2009/04/24)
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- Synthesis of 4-substituted 3,5-dicyano-2,6-piperidinediones using lithium nitride as a convenient source of ammonia
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A simple and efficient one-pot synthesis of 4-substituted-3,5-dicyano-2,6-piperidinediones was achieved in good yields via the three-component reaction of aldehyde or ketone, ethyl cyanoacetate, lithium nitride (Li3N) as a convenient source of ammonia in MeOH.
- Wu, Liqiang,Yang, Chunguang,Yang, Liming,Yang, Lijuan
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experimental part
p. 977 - 982
(2009/09/30)
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- PROCESS FOR THE PREPARATION OF GABAPENTIN HYDROCHLORIDE
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A process for preparation of gabapentin hydrochloride by converting 1,5-dicyano-2,4-dioxo-3-azaspiro[5,5]-undecane into 1,5-diaminoformyl-2,4-dioxo-3-azaspiro[5,5]-undecane at a temperature of 65°C to 85°C in the presence of a strong acid, and then carrying out Hofmann rearrangement under an alkaline condition. The starting material of the process is readily available. The process is simple, and can reduce the purification procedure of intermediates, reduce production cost, and obtain product with higher purity.
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Page/Page column 5; 6
(2008/12/06)
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- Antiarthritic and suppressor cell inducing activity of azaspiranes: Structure-function relationships of a novel class of immunomodulatory agents
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Spirogermanium (1;8,8-diethyl-N,N-dimethyl-2-aza-8-germaspiro[4.5]decane-2-propanamin e dihydrochloride) is a potent cytotoxic agent in vitro which has demonstrated limited activity in experimental animal tumor models. Subsequently, it has been reported that spirogermanium has antiarthritic and suppressor cell-inducing activity. We have synthesized a series of substituted 8-hetero-2-azaspiro[4.5]decane and 9-hetero-3-azaspiro[5.5]undecane analogues of spirogermanium to identify the heteroatom requirements for in vivo antiarthritic and suppressor cell-inducing activity. This structure-activity relationship study has identified that appropriately substituted silicon and carbon analogues of spirogermanium retain both antiarthritic and immunosuppressive activity, with the 8,8-dipropyl (carbon) analogue being among the most active. Following the identification of N,N-dimethyl-8,8-dipropyl-2-azaspiro[4,5]decane-2-propanamine dihydrochloride (9) as more active analogue than spirogermanium, a series of 8,8-dipropyl analogues with various amine substituents were synthesized. A number of these analogues had activity similar to that of 9. A correlation between activity in the adjuvant arthritic rat and the ability to induce suppressor cells (r = 0.894, p0.001) suggests an association between the two pharmacologic effects. While the precise biochemical mechanism(s) for the pharmacological activity is unclear, these data suggest that compounds within this series, e.g., N,N-dimethyl-8,8-dipropyl-2-azaspiro[4.5]decane-2-propanamine dihydrochloride, may provide effective therapy in diseases of autoimmune origin and/or the prevention of rejection in tissue transplantation.
- Badger,Schwartz,Picker,Dorman,Bradley,Cheeseman,DiMartino,Hanna,Mirabelli
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p. 2963 - 2970
(2007/10/02)
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