Preparation method of N, N, N ', N'-tetra-n-butyl-1, 6-hexamethylenediamine
A technology of tetra-n-butyl and hexamethylenediamine, applied in the preparation of amino-substituted functional groups, organic chemistry, etc., can solve the problems of poor selectivity and easy generation of by-products, and achieve high selectivity, high selectivity, and high yield Effect
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[0021] The preparation method of N,N,N',N'-tetra-n-butyl-1,6-hexanediamine of the present invention comprises the following steps: adding a dihalogenated dihalogen to a solution comprising a selective reagent, di-n-butylamine and a solvent; Hexane, di-n-butylamine and dihalohexane are subjected to substitution reaction to obtain N,N,N',N'-tetra-n-butyl-1,6-hexanediamine, wherein the dihalohexane The alkane is one of 1,6-difluorohexane, 1,6-dichlorohexane, 1,6-dibromohexane, and 1,6-diiodohexane, and the selective reagent is non-philic Nuclear organic base.
[0022] The substitution reaction of the di-n-butylamine is to replace the hydrogen atom attached to the nitrogen atom of the di-n-butylamine by the hydrocarbyl moiety of the haloalkane in the presence of a selective reagent. The chemical reaction equation of the present invention is shown in the following formula, wherein X represents a halogen.
[0023]
[0024] In one embodiment, the addition rate of the dihalohexan...
Embodiment 1
[0039] Add di-n-butylamine and diisopropylethylamine with a molar ratio of 1:1 and 100 ml of acetonitrile to a glass reactor, pass nitrogen into the reactor to remove the oxygen in the solution, and then run at 250 rpm / The solution in the reactor was stirred at a rotating speed of 10 minutes, and then 1,6-dibromohexane was added dropwise to the reactor at an addition flow rate of 0.07 wt% / min, so that the acetonitrile and 1,6-dibromohexane were mixed. The weight ratio is 16.6:1, the temperature at which the 1,6-dibromohexane is added dropwise is 30°C, and after the dropwise addition is completed, the reaction vessel is controlled to carry out the substitution reaction at a reaction temperature of 30°C and a pressure of 1 atmosphere, and The reaction time for this substitution reaction was 24 hours. After the reaction was completed, the solution in the reactor was distilled to obtain a crude product of mono-N,N,N',N'-tetra-n-butyl-1,6-hexanediamine. The crude product was extr...
Embodiment 2
[0042] The preparation method is the same as in Example 1, but the reaction time of the substitution reaction is changed to 120 hours to obtain the final product N,N,N',N'-tetra-n-butyl-1 with a selectivity of 96% and a yield of 96%, 6-Hexanediamine.
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