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Chemical Structure| 779-14-6 Chemical Structure| 779-14-6

Structure of 779-14-6

Chemical Structure| 779-14-6

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Product Details of [ 779-14-6 ]

CAS No. :779-14-6
Formula : C14H13Cl
M.W : 216.71
SMILES Code : CC1=CC=C(C(Cl)C2=CC=CC=C2)C=C1
MDL No. :MFCD00972764

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Application In Synthesis of [ 779-14-6 ]

* 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 [ 779-14-6 ]

[ 779-14-6 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 20845-34-5 ]
  • [ 74-83-9 ]
  • [ 779-14-6 ]
  • [ 110-16-7 ]
  • [ 35620-67-8 ]
YieldReaction ConditionsOperation in experiment
With sodium hydroxide; In 5,5-dimethyl-1,3-cyclohexadiene; diethyl ether; ethanol; water; acetone; toluene; Petroleum ether; EXAMPLE II 285 g (2.2 mole) of 1-methylpiperidin-2-ylmethanol in 1.25 liters of anhydrous xylene are added drop-wise under reflux to a solution of 216.5 g (1 mole) of p-methyl-a-phenylbenzyl chloride dissolved in 1.25 liters of anhydrous xylene. When the addition is completed, the mixture is refluxed for another 4 hours. The precipitate consisting of 1-methylpiperidin-2-ylmethanol hydrochloride is filtered off. The filtrate is washed with water until it is neutral and dried with sodium sulphate. The xylene is distilled off and the residue is dissolved in a mixture of 500 ml of ethanol and 2 liters of diethyl ether. 100 g of maleic acid, dissolved in 250 ml of ethanol, are added under stirring. The precipitate, consisting of 1-methyl-2-[(p-methyl-a-phenylbenzyl)oxymethyl]piperidine maleate is filtered off and digested in acetone. The salt is filtered off again and dissolved in water. The solution is made alkaline with 2 N sodium hydroxide and extracted with diethyl ether. The extract is dried over sodium sulphate and the ether is evaporated. The residue, consisting of 83 g of the base, is dissolved in 900 ml of acetone and then methyl bromide is introduced with stirring at room temperature until no further precipitation takes place. 1800 ml of petroleum ether (boiling range 40°-60° C.) are added to effect complete precipitation of the methobromide formed. The precipitate is filtered off and dried over sodium sulphate. To remove p-methyl-a-phenyl-benzylalcohol, present as a contaminant, the product is refluxed for 6 hours in 1000 ml of toluene. Filtration yields 90 g of 1,1-dimethyl-2[[(p-methyl-a-phenylbenzyl)oxy]methyl]piperidinium bromide. Melting point 180.2°-180.9° C.
 

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