A NEW METHOD OF SYNTHESIS OF P-NITRO-N-METHYLAMINE

摘要

P-nitro-N-methylamine can be used as propellant Stabilizer, an extensively used organic intermediate and as norm substance. It is studied by the new technology of synthesis of P-nitro-N-methylamine with P-nitrochlorobenzen (I) used as raw material through sulfonation amination and hydrolyzation in this paper. The experimental results showed that reaction conditions for sulfonation with 65% oleum to give 2-chloro-5-nitrobenzensulfonic acid were that molar ratio SO3 to I is (1.4-1.5): 1 at 120-125 °C for 3-5h. 2-chloro-5-nitrobenzensulfonic acid sodium salt( II) is obtained by neutralization with NaOH. Reaction conditions for amination with 25-30% methylamine to give N-methyl-4-nitrobenzene-2-sulfonic sodium salt(III) was that molar ratio methylamine to II is 30:1 at 82 °C for 7h.. PNMA was prepared by III in the presence of 25% sulphuric acid at 102°C for 4-5h. Under these conditions, the reaction overall yield was up to 78.5%.