SU565033A1 - Monodiazotized melamin as intermadiate for obtaining ammeline - Google Patents

Description

one

The invention relates to the synthesis of a new melamine derivative monodiazated melamine, which can be used as an intermediate product for the production of agricultural-grade ammeline.

Methods for the preparation of ammeline are known using various derivatives of simm as intermediates. triazine, for example cyanuric acid, melamine 2, or 2, 4-diamino-6-chloro-cmlsh. triazine 3.

However, when using these derivatives simm. The triazine process must be carried out at high temperatures and pressures of 1. The target product is obtained with an insufficiently high yield (70-80%) of 1, 3 or insufficient purity, and therefore requires an additional stage of its purification 1, 2.

Offered as an intermediate product in the synthesis of ammeline, monodisaturated melamine allows to obtain the target product in almost quantitative yield, of high quality, under mild conditions that do not require heating and pressure.

The method of obtaining monodiazoated melamine formula

2

..H2

T T

t vr

V © e

Kg nyo :,

based on the reaction of diazotization of amino compounds and is that melamine is reacted with sodium nitrite in concentrated sulfuric, acetic or phosphoric acids or mixtures thereof.

The products are isolated by conventional means, for example, diluting the reaction mixture with organic solvents which are miscible with concentrated acids, for example acetone, ethanol, methanol.

Example 1. 0.7 g (0.01 mol) of sodium nitrite is dissolved at room temperature in 12 ml of concentrated sulfuric acid.

(d 1.84 g / cm) and gradually poured to a solution of 1.26 g (0.01 mol) of melamine in 25 ml of concentrated acetic acid. Stirring is carried out for 2 hours. Then the reaction mixture is poured with vigorous cooling and stirring into dry acetone. The product is filtered off, washed with dry acetone and a white powder is obtained which is insoluble in organic solvents. The yield is 97-98%. The content of azo groups, determined volumetrically by the nitrogen emitted during decomposition, is 11.9%, which corresponds to the theoretical amount.

Found,%: C 15.20; H 2.25; N 42.00.

Calculated,%: C 15.32; H 2.13; N 41.70.

Example 2. To a solution of 10 ml of concentrated sulfuric acid (, 84 g / cm) and 0.7 g (0.01 mol) of sodium nitrite in 50 ml of phosphoric acid (fi (l, 65 g / 1 cm), powdered 1.26 g (0.01 mol) of melamine and stirred for 2 hours at room temperature. Isolation of the final product is carried out as in Example 1. Yield 97-98%.

Upon hydrolysis of the resulting diazo compound, nitrogen is released with a yield of 99.5%, calculated for the monodiazo compound, and ammeline is obtained with a yield of 99.0%.

Claims (3)

1. V.A. Halperin et al. Pyrolysis of Cyanuric Acid under the Pressure of Emit Gases, Proceedings of the Research and Design Institute of the Nitrogen Industry and Organic Synthesis Products, 1972, N ° 16, p. 48. 2. Karlik VM, et al., Kinetics of triazine hydrolysis. Hydrolysis of melamine, ammelia, ammelide, ZhVHO them. D.I. Mendeleev, 1971, JMb 1. p. 116. 3.Tuka R. et al., Otxzymywanil Amelidu i Amclinu v Statiic czystum., Chcm. Stosowana A., 1970, T., c. 339.