SU798102A1 - Method of combined preparation of n,n,n-tribenzylhexahydrotriazine-1,3,5 and n-methylbenzylamino-n'-benzyliminomethylene - Google Patents

Description

one

The invention relates to the method for obtaining a mixture of N, N, N -tribenzylhexagyarotriazin-1, 3.5 and N -methylbenzylamino-N -benzylminomethylene, which is used as an acid corrosion inhibitor for metals.

A known method of obtaining a mixture of M M f N -tribenyl hexahydrotriazine-1, 3.5 and M - lethylbenzylamino-N-benzyliminomethylene by reacting bisylamine with hexamethylenetetram at 180-200 0. The mixture yields 75% at a conversion of 8O% over the marine benzylamine ij.

The disadvantages of this method are the high process temperature and the use of relatively scarce raw material benzylamine.

The purpose of the invention is to simplify the process, eliminating the use of high process temperatures and scarce raw materials.

The goal is achieved by obtaining a mixture of N, N, N -tribenzylhexahydrotriazin-1, 3.5 and N-methylbenzylamino-N -benzylminomethylene by reacting benzyl chloride with freshly prepared: 2 O-25% - ammonia solution in 5-15% - a formaldehyde aqueous solution at a molar ratio of 1: 1.1 -1.15 at 20-30 C.

The proposed method allows the process to be carried out at lower temperatures (20-30 C) than with the known (18 O-200 C), and to use a more accessible raw material - benzyl chloride.

In addition, the mixture of M, N, N -tribenzylhexahydro-triazine-1, 3.5 and N-methylbenzylamino-W-enzyliminomethylene, obtained by the proposed method, has a higher anticorrosion activity than the mixture obtained by a known method.

The resulting mixture of N, K /, N1-tribenzylhexahydro-triazine-1, 3.5 and N-methylbenzylamino-N-benzylminomethylene is a clear syrupy liquid with an ammonia odor; specific gravity 1, О5 n 1,5825; viscosity 150–200 cCr; Good rdsgvornma in almost all organic solvents. According to the mass and IR spectra, it contains about 607O% N, W, N -tribenylhexagndrotria .zina-1,3,5 and about 3A-4O% N-methylbenyl-amino-N-benzylminomethylene; 3%). N .. H, N -tribenes1hexahydrothyzine “.1,3,5 can be easily separated out of the mixture when cooled to 10–15 ° C and purified by recrystallization from alcohol or dry acetoma (yield 9O-95%). After purification, it is a white crystalline product with a melting point of 43-46 0, easily soluble in benzene, xylene, acetal, acids, worse - in alcohols, insoluble in water and alkalis. From the residue after isolation of N, N of C-ch-ribenyl hexa-hyarotriazine-1,3,5 by distillation in vacuum, the fraction with bp 13 and -14 ° C and mm), (, O379 t) p 1.5640, corresponding to the elemental analysis of N "mvtilbanylamino-H-bena and aminomethylene. Cement analysis: Calculated,%: C 80.5; H 7.55j N 11; 95.C, gWo% Found,%: C 79, H 7.97; N11.59. The resulting mixture of N, M, -tribenyl-xylahydrothyryazine-1,3,5, and N. . 7 24 Example -1. In a four-necked flask equipped with a stirrer, thermometer, bubbler and reflux condenser, 165 ml of a 10% aqueous solution of formaldehyde are placed (a 10% aqueous solution of paraformaldehyde can be used). At 20c, gaseous ammonia is passed into the solution until saturation (ammonia content is 25%). At the same time, a rise in temperature to 30 ° C is observed. Then, 63.2 g of benzyl chloride is added with stirring for 40 minutes at the same temperature. The mixture is heated to 7 ° C, after which the stirrer is stopped, the reaction mixture is settled and the aqueous layer is drained. The yield of N, N, M -tribenzylhexahydrotriaina-1, 3.5 and M-methylbenzylamino-N -benzyliminomethylene is about 95% (56 g of a thick syrupy liquid of light yellow color). The composition is based on mass spectral analysis: N, N, N -tribenzylhexahydrotriazin-1, 3.5 68, N-methylbenzylamino-N -benzylminomethylene 31%. Example 2. Similar to example 1, except that the content of ammonia in an aqueous solution of formaldehyde is 2 O%. Received 56 g thick syrupy liquid light yellow color. Yield 95%. The composition according to the mass spectral analysis: N, M, N-tribenyl hexahydrotriain-1, 3.5 6O, N-methylbenzylamino-N-benzyliminomethylene 38%. The table presents the results of testing a mixture of N, N, N -tribenzylhexahidrotriazina-1, 3.5 and N-metkpbenzylamio N -benzyliminomethylene, obtained by the proposed method, and a mixture obtained in a known manner ,,. as inhibitors of acid corrosion.

semi-forward

435 2O4 380

The mixture obtained in a known manner 183,9 147 214

335 222

183

172

87

Claims (1)

5 O 12 O, 5 94.8 5 O, 7 42.5 5 7981 O The invention The method of joint production of N i N. N -tribenyl hexagnarotriaine-1,3.5 m,. wi and N are methylbenzylamino-Jv enyl methyl 5 methylene, characterized in that, in order to simplify the process, benzyl chloride is subjected to combined action with freshly prepared 20-25% ammonia solution in a 5-15% aqueous solution of formaldehyde itpH mo26 L In the treatment of benzyl chloride in formaldehyde 1-1,, 15 at a temperature of 20-ZO S. ... The sources of information, „„, received in-vnmanne during examination v 1. Murashova, OP and others. Study of the composition and structure of the products of the interaction of benzstamine in hexamethylenetetramine. -ZPH, 1975, № 8 t.48, p. 18O2 (prototype).