A kind of synthetic method of n-methyltyramine hydrochloride
A technique for the synthesis of methyltyramine hydrochloride, which is applied in the fields of chemical instruments and methods, the preparation of amino hydroxyl compounds, and the preparation of carboxylic acid amides, and can solve the problems of high equipment loss and post-processing costs, environmental and operator injuries, Eye and soft tissue sensitization and other problems, achieving the effect of low synthesis cost, low environmental pollution, and simple and easy treatment
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Embodiment 1
[0029] Condensation reaction: Dissolve 153g of p-hydroxyphenylacetic acid in 200mL of dichloromethane, add dropwise 120g of thionyl chloride at 0°C, stir at reflux for 5 hours until the reaction is detected by TLC, then drop into 800mL of 40% methylamine aqueous solution under cooling , dripping and insulated and stirred for 2 hours, suction filtered, and washed the filter cake with water to obtain the intermediate of 150g yellow solid;
[0030] Reduction reaction: add 1000mL tetrahydrofuran into a 10L reaction flask, add the above-mentioned intermediate, add 76g sodium borohydride at room temperature, and then add 133g aluminum chloride in batches, after completion, reflux and stir overnight. After the reaction was detected by TLC, the reaction solution was slowly poured into 2000 mL of 6 mol / L dilute hydrochloric acid, and after stirring for 1 hour, an aqueous solution of sodium hydroxide was added dropwise to pH = 7, and after stirring for 1 hour, it was filtered, separated,...
Embodiment 2
[0032] Condensation reaction: Dissolve 76.5g of p-hydroxyphenylacetic acid in 100mL of acetone, add 90g of thionyl chloride dropwise at 0°C, reflux and stir for 5 hours until the reaction is detected by TLC, then drop into 400mL of 40% methylamine aqueous solution under cooling, After dropping, keep stirring for 2 hours, filter with suction, rinse the filter cake with water, and obtain 75 g of a yellow solid intermediate;
[0033] Reduction reaction: add 500mL of toluene into a 5.0L reaction flask, add the above intermediate, add 38g of sodium borohydride at room temperature, and then add 66.5g of aluminum chloride in batches, after completion, reflux and stir overnight. After the reaction was detected by TLC, the reaction solution was slowly poured into 1000 mL of 6 mol / L dilute hydrochloric acid. After stirring for 1 hour, aqueous sodium hydroxide solution was added dropwise to pH = 7. After stirring for 1 hour, it was filtered, separated, and the dried tetrahydrofuran The l...
Embodiment 3
[0035] Condensation reaction: Dissolve 153g of p-hydroxyphenylacetic acid in 200mL of chloroform, add 120g of thionyl chloride dropwise at 0°C, stir at reflux for 5 hours until the reaction is detected by TLC, then drop into 800mL of 40% methylamine aqueous solution under cooling , dripping and insulated and stirred for 2 hours, suction filtered, and washed the filter cake with water to obtain the intermediate of 150g yellow solid;
[0036] Reduction reaction: add 1000mL tetrahydrofuran into a 10L reaction flask, add the above-mentioned intermediate, add 76g sodium borohydride at room temperature, and then add 266g aluminum chloride in batches, after completion, reflux and stir overnight. After the reaction was detected by TLC, the reaction solution was slowly poured into 2000 mL of 6 mol / L dilute hydrochloric acid, and after stirring for 1 hour, an aqueous solution of sodium hydroxide was added dropwise to pH = 7, and after stirring for 1 hour, it was filtered, separated, and ...
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