- Method for synthesizing trans-cyclohexyldiamine
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The invention discloses a method for synthesizing trans-cyclohexyldiamine. The method comprises the following steps: by using epoxy cyclohexane as the raw material, carrying out ring opening with ammonia water, adding sulfuric acid for dewatering and salification, adding free alkali, carrying out ring opening with ammonia water, and distilling to obtain the trans-cyclohexyldiamine. The method has the advantages of high repetitiveness of the synthesis route, and simple and accessible raw materials, and provides an alternative scheme for obtaining the trans-cyclohexyldiamine pure product.
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Paragraph 0013; 0014; 0015
(2017/08/29)
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- Preparation method of 1,2-cyclohexylenediamine
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The invention provides a preparation method of 1,2-cyclohexylenediamine. The method adopts a one-step technology to prepare 1,2-cyclohexylenediamine. The method is simple, and simple, easily available and cheap 2-aminocyclohexanol is adopted as a raw material, so the production cost is effectively reduced, and large-scale industrial production is facilitated.
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Paragraph 0024; 0025
(2017/01/02)
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- CYCLOHEXANEDIAMINE COMPOUNDS AND METHODS FOR THEIR PREPARATION
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The present invention provides processes for the preparation of cyclohexanediamine compounds of formula Ia and intermediates thereof. The compounds are useful as Syk kinase inhibitors and in various pharmaceutical compositions, and particularly useful for treating conditions mediated at least in part by Syk kinase activity.
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Paragraph 0099
(2014/10/04)
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- Efficient chiral resolution of (±)-cyclohexane-1,2-diamine
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A novel and efficient method has been developed for the chiral resolution and separation from cis-cyclohexane-1,2-diamine of (±)-cyclohexane-1,2- diamine, which reacts with xylaric acid, a substitute for tartaric acid. This method provides (1R,2R)-cyclohexane-1,2-diamine, and (1S,2S)-cyclohexane-1,2- diamine and cis-cyclohexane-1,2-diamine in good yield with high optical purity.
- Gao, Chuan-Zhu,Wang, Tian-Shuai,Chen, Jia,Fei, Fan,Zhang, Yan,Yang, Bo
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p. 490 - 492
(2014/11/08)
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- Direct amination of bio-alcohols using ammonia
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A slightly adapted catalyst system has been successfully applied in the direct amination of primary and secondary alcohols. Moreover, the applicability to diols has been shown, giving high selectivity towards the primary diamines. It was found that the Ru/P ratio as well as the amount of ammonia used are highly important in this system, especially for higher substrate loadings. The catalyst was employed on a larger batch scale for the conversion of isomannide to the corresponding diamine. Additionally, it was shown that the catalyst is stable for at least six consecutive runs. No significant loss of activity and selectivity was observed.
- Pingen, Dennis,Diebolt, Olivier,Vogt, Dieter
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p. 2905 - 2912
(2013/10/21)
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- Synthesis of cis-TMCDA: Optimization and characterization of a key intermediate
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We report optimized synthetic procedures to cis-TMCDA and cis-cyclohexane-1,2-diamine. Our new two-step approach is an efficient and low-cost method for synthesizing the ligand cis-TMCDA. In the preparation of cis-cyclohexane-1,2-diamine, the crystallization of the unexpected intermediate cis-cyclohexane-1,2-diammonium hydrogensulfate ethylsulfate made the subsequent reactions easier in their workup, as nickel(II) chloride impurities were eliminated.
- Eckert, Prisca K.,Schill, Verena,Strohmann, Carsten
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experimental part
p. 634 - 637
(2011/11/01)
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- A new approach to enantiomerically pure bis-imidazoles derived from trans-1,2-diaminocyclohexane
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Racemic as well as enantiomerically pure trans-1,1′-(cyclohexane-1,2-diyl)bis(imidazole N-oxides) were prepared from trans-cyclohexane-1,2-bis(methylidenamine) and 1,2-dione monooximes (α-hydroxyiminoketones). The enantiomeric purity of selected products was determined by means of 1H NMR spectroscopy in the presence of (+)-(R)-(tert-butyl)(phenyl)phosphonothioic acid as a chiral solvating agent. Deoxygenation by treatment with Raney-nickel led to the corresponding chiral bis-imidazoles.
- Mucha, Paulina,Mloston, Grzegorz,Jasinski, Marcin,Linden, Anthony,Heimgartner, Heinz
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p. 1600 - 1607
(2008/12/21)
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- The stereospecific addition of hydroxylamines to α,β-unsaturated sulfones, nitriles and nitro compounds
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N-Alkyl hydroxylamines have been shown to undergo a highly stereospecific cis addition to α,β-unsaturated sulfones, nitriles and nitro compounds.
- O'Neil, Ian A.,Cleator, Ed,Southern, J. Mike,Bickley, Jamie F.,Tapolczay, David J.
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p. 8251 - 8254
(2007/10/03)
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- A diamine-exchange reaction of dihydropyrazines
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Dihydropyrazines reacted with 1,2-diamines to form tetraazadecalins as intermediates, and then the reaction proceeded forward to dissociate into alternate dihydropyrazine and diamine, or backward to dissociate into the starting materials in certain equilibrium. The product distribution is controlled by diamine-exchange equilibrium reaction. The various equilibrium reactions were analyzed by NMR spectroscopy.
- Yamaguchi, Tadatoshi,Ito, Shigeru,Iwase, Yukiko,Watanabe, Kenji,Harano, Kazunobu
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p. 1677 - 1680
(2007/10/03)
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- Diastereo- and enantioselective synthesis of vicinal diamines via aza-Michael addition to nitroalkenes
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The asymmetric synthesis of protected 1,2-diamines 4 by aza-analogous Michael addition of (-)-(2S,3R,4R,5S)-1-amino-3,4-dimethoxy-2,5-bis(methoxymethyl)pyrrolid ine (ADMP) to nitroalkenes 1 in good overall yields and high enantiomeric excesses (ee = 93-96%) is described. The auxiliary constitutes a novel chiral equivalent of ammonia and is removed under reductive N-N bond cleavage with Raney nickel, which also reduces the nitro group. The absolute configuration was determined by NMR-spectroscopic methods and polarimetry.
- Enders, Dieter,Wiedemann, Juergen
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p. 1443 - 1450
(2007/10/03)
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- Antineoplastic platinum (IV) complexes and compositions
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New substantially isomerically pure tetrahalo (1,2-diaminocyclohexane) Pt (IV) complexes having antineoplastic activity are disclosed.
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- Synthesis of platinum (IV) antineoplastic agents
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There is provided a method of synthesizing tetrachlorocyclohexanediammine platinum (IV) compounds in high purity and yield, the level of purity being suitable for pharmacological use. The compounds produced by this process have antineoplastic agents against tumor cells resistant to cis-platinum.
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