1,4-Amino-N,N-dimethylaniline,dihydrochloride synthesis

Yield:536-46-9 97.3%

Reaction Conditions:

with water;sodium hydroxide in toluene at 20 - 40; for 2 h;Heating;Temperature;

Steps:

1-3 A method for preparing N,N-dimethyl-p-phenylenediamine hydrochloride, comprising the steps of:

(1) taking 1 mole of p-nitrochlorobenzene dissolved in 500ml of toluene to obtain a solution A;(2) taking 1.2 moles of dimethylamine hydrochloride dissolved in 200ml of water, adding solution A;(3) 20 to 25 ° C, while stirring, add 1.25 moles of 15% aqueous sodium hydroxide solution to the above solution, and heat up to 40 °C, 0.8 ml of 15% aqueous sodium hydroxide solution was added dropwise in 30 minutes, and then the reaction was kept for 90 minutes;(4) standing, phase separation, toluene layer plus active nickel catalyst, hydrogenation reduction;(5) filtering and separating the catalyst;The toluene layer is passed through a hydrogen chloride gas,Obtaining N,N-dimethyl-p-phenylenediamine hydrochloride precipitate;(6) centrifugation,N,N-dimethyl-p-phenylenediamine hydrochloride 204g,The content is 99.6%,The yield was 97.3% (based on p-chloronitrobenzene).

References:

CN109970569,2019,A Location in patent:Paragraph 0027-0050