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Chemical Structure| 56496-16-3 Chemical Structure| 56496-16-3

Structure of 56496-16-3

Chemical Structure| 56496-16-3

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Product Details of [ 56496-16-3 ]

CAS No. :56496-16-3
Formula : C10H20ClN
M.W : 189.73
SMILES Code : C1CCCC[N+]12CCCCC2.[Cl-]
English Name :6-Azaspiro[5.5]undecan-6-ium chloride
MDL No. :MFCD06637668

Safety of [ 56496-16-3 ]

Application In Synthesis of [ 56496-16-3 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 56496-16-3 ]

[ 56496-16-3 ] Synthesis Path-Downstream   1~2

  • 1
  • [ CAS Unavailable ]
  • [ 628-76-2 ]
  • [ 56496-16-3 ]
YieldReaction ConditionsOperation in experiment
97% With sodium hydroxide at 100℃; for 5h; 7 Example 7: Synthesis of 6-azoniaspiro[5.5]undecane chloride (0091) A mixture of 8.6 g (10 ml, 100 mmol, 99% purity) piperidine, 14.4 g (13 ml, 100 mmol, 98% purity) 1,5-dichloropentane and 8.0 g (100 mmol, 98% purity) of a 50 wt% sodium hydroxide solution was heated to 100 °C under reflux for 5 hours, then 100 ml of isopropanol added and the heterogeneous mixture left to cool off. Next, precipitated NaCl was filtered off and the solvent evaporated, then the residue taken up in circa 20-25 ml of hot ethanol and the product precipitated via the addition of 150 ml of methyl-tert-butyl ether. The product was filtered off, washed with some more methyl-tert-butyl ether and dried in vacuo to give 18.4 g (97 mmol, 97% yield) of white, powdery 6- azoniaspiro[5.5]undecane chloride.
  • 2
  • [ 628-76-2 ]
  • [ 56496-16-3 ]
YieldReaction ConditionsOperation in experiment
361 g With ammonia; triethylamine In ethanol at 70℃; 10 General procedure: (1) First, add 409g of an organic solvent (anhydrous acetonitrile), 607g (6mol) of an acid-binding agent (triethylamine), and 36g (2.1mol) of liquid ammonia to a high-pressure reactor in sequence, raise the temperature to 70°C, and then add 508g (4mol) of a dihalogenated alkane (1,4-dichlorobutane) dropwise at a rate of 600g/h after the temperature stabilizes;Then, at 70°C and 0.02MPa pressure for 8h, and after returning to room temperature, 1548.3g of halogenated bispirocyclic quaternary ammonium salt reaction solution was obtained;(2) 415g (6.1mol) of organic base (sodium ethoxide) was added to the halogenated bispirocyclic quaternary ammonium salt reaction solution obtained in step (1), the system pH was 11, and deamination and dehydration were carried out at normal pressure at 80 for 5 hours, and then the solvent was continuously removed under reduced pressure at -0.098MPa and 120 for 10 hours to obtain 665.7g of solid mixture.(3) the solid mixture obtained in step (2) is fully dissolved with 400g of organic solvent (anhydrous acetonitrile), and then filtered to obtain a solution of the bispirocyclic quaternary ammonium salt, and crystallized at a low temperature of -15°C. The obtained crystals are fully dissolved in 402g of organic solvent (anhydrous acetonitrile), and then recrystallized at a low temperature of -15°C, and then filtered to obtain high-purity bispirocyclic quaternary ammonium salt crystals. The filtrate is recovered and can be used as an organic solvent for the preparation of the next batch of bispirocyclic quaternary ammonium salts; the bispirocyclic quaternary ammonium salt crystals are vacuum dried at 120°C for 8 hours to obtain 312g (1.9mol) of the bispirocyclic quaternary ammonium salt.
 

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