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Chemical Structure| 4204-16-4 Chemical Structure| 4204-16-4

Structure of 4204-16-4

Chemical Structure| 4204-16-4

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Product Details of [ 4204-16-4 ]

CAS No. :4204-16-4
Formula : C7H16N2
M.W : 128.22
SMILES Code : CC1CNCC(C)N1C

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Application In Synthesis of [ 4204-16-4 ]

* 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 [ 4204-16-4 ]

[ 4204-16-4 ] Synthesis Path-Downstream   1~2

  • 1
  • [ 50-00-0 ]
  • sodium dihydrogen phosphite [ No CAS ]
  • [ 639068-43-2 ]
  • [ 10294-56-1 ]
  • [ 4204-16-4 ]
YieldReaction ConditionsOperation in experiment
With sodium hydroxide; trifluoroacetic acid; In 1,4-dioxane; dichloromethane; water; PREPARATION 77 cis 3,4,5-Trimethylpiperazine To a solution of 1-(1,1,dimethylethoxycarbonyl)-cis-3,5-dimethylpiperazine (PREPARATION 76, 4.28 g) in dioxane (100 ml) is added 1M sodium dihydrogen phosphite (100 ml, made by mixing equal volumes of 2M sodium hydroxide and 2M phosphorous acid) followed by the addition of formalin solution (37percent, 16 ml). The mixture is heated at 65° for 2.5 hr and extracted with methylene chloride. The organic phase is washed with water and saline, dried over sodium sulfate and concentrated to ca. 50 ml. The remaining methylene chloride and dioxane are removed by distillation leaving 4.3 beta of residue in the distillation flask. This material is dissolved in methylene chloride (40 ml), cooled to 0°, and trifluoroacetic acid (14.5 ml) is added. The mixture is stirred for 1.25 hr and sodium hydroxide (11.3 g) in water (30 ml) is added. The phases are separated and the aqueous phase is extracted with additional methylene chloride. The total combined organics are dried over magnesium sulfate and concentrated by distillation to give a mixture of the title compound and residual starting material. On standing the mixture partially crystallizes. Filtration and washing with ethyl ether gives the title compound, NMR (chloroform-d) 3.09, 2.67, 2.39, 1.16 delta.
  • 2
  • [ 639068-43-2 ]
  • [ 4204-16-4 ]
 

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