Method for preparing tetramethyl ammonium bromide
A technology of tetramethylammonium bromide and demethylation, which is applied in chemical instruments and methods, preparation of amino compounds, preparation of organic compounds, etc., can solve problems such as low methyl bromide concentration, large equipment investment, and environmental impact, and achieve The process is simple and easy, the cost is low, and the effect of good competitiveness
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Embodiment 1
[0025] Add 600ml of absolute ethanol to a 1000ml stirred three-neck flask, and cool to 20°C.
[0026] Add 122g of p-methoxytoluene to the acetic acid solution of hydrogen bromide for demethylation reaction. The methyl bromide gas generated by the reaction is first passed into 200ml of 20% NaOH aqueous solution, and then successively passes through the adsorption device with a diameter of 1cm and a height of 5cm, which is filled with granular activated carbon fillers. The column and the adsorption column with a diameter of 3cm and a height of 10cm and anhydrous calcium chloride filler inside are filled with pure and dry methyl bromide gas that removes residual moisture into the above-mentioned anhydrous ethanol that is stirring until the demethylation reaction is completed.
[0027] Put 500g of 30% trimethylamine aqueous solution in a 1000ml three-neck bottle, heat it to 50°C, and pass the released trimethylamine gas into an adsorption column with a diameter of 3cm and a height ...
Embodiment 2
[0030] Add 600ml of absolute ethanol into a 1000ml stirred three-neck flask, and cool to 10°C.
[0031] Add 150g of p-methoxyacetophenone to the acetic acid solution of hydrogen bromide for demethylation reaction. The methyl bromide gas generated by the reaction is first passed into 200ml of 10% NaOH aqueous solution, and then sequentially through the 1cm in diameter and 5cm in height, filled with granular activated carbon filler. The adsorption column and the adsorption column with a diameter of 3 cm and a height of 10 cm are filled with granular anhydrous calcium chloride filler, and the pure dry methyl bromide gas that removes residual moisture is passed into the above-mentioned absolute ethanol that is stirring until the demethylation reaction is completed.
[0032] Put 200g of trimethylamine hydrochloride in a 1000ml three-neck bottle, slowly add 600ml of 20% NaOH aqueous solution dropwise, and control the temperature not to exceed 50°C during the dropwise addition. The t...
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