2,4,6-TRIS[BIS(METHOXYMETHYL)AMINO]-1,3,5-TRIAZINE synthesis

Yield:-

Reaction Conditions:

with nitric acid in water; pH=1.5 - 3.8 at 45 - 55; for 1.5 h;Product distribution / selectivity;

Steps:

8; 9; 10; 11; 12 Example 8
Production of hexamethoxymethylol melamine Example 8 Dry hexamethylol melamine from Example 1 was dosed into a suitable mixing vessel equipped with heating, cooling and mixing equipment. To 1 mole of hexamethylol melamine 12 moles of methanol were added, the pH was set to 1.5-1.9 with nitric acid and it was etherified at 45°C for 1.5 hours. Then the reaction mixture was neutralized with a NaOH solution and the volatile components were vacuum-distilled off. The properties of the product hexamethoxymethylol melamine are given in Table 1. Example 9; Dry hexamethylol melamine from Example 1 was dosed into a suitable mixing vessel equipped with heating, cooling and mixing equipment. To 1 mole of hexamethylol melamine 9 moles of methanol were added, the pH was set to 3.6-3.8 with nitric acid and it was etherified at 55°C for 1.5 hours. Then the reaction mixture was neutralized with a NaOH solution and the volatile components were vacuum-distilled off. The properties of the product hexamethoxymethylol melamine are given in Table 1.; Comparative Example 10; Hexamethylol melamine from the Comparative Example 5 was dosed into a suitable mixing vessel equipped with heating, cooling and mixing equipment. To 1 mole of hexamethylol melamine 12 moles of methanol were added, the pH was set to 3.6-3.8 with nitric acid and it was etherified at 55°C for 1.5 hours. Then the reaction mixture was neutralized with a NaOH solution and the volatile components were vacuum-distilled off. The properties of the product hexamethoxymethylol melamine (HMMM) are given in Table 1.; Comparative Example 11; Hexamethylol melamine from the Comparative Example 5 was dosed into a suitable mixing vessel equipped with heating, cooling and mixing equipment. To 1 mole of hexamethylol melamine 30 moles of methanol were added, the pH was set to 1.5-1.9 with nitric acid and it was etherified at 45°C for 1.5 hours. Then the reaction mixture was neutralized with a NaOH solution and the volatile components were vacuum-distilled off. The properties of the product hexamethoxymethylol melamine (HMMM) are given in Table 1.; Example 12; Dry hexamethylol melamine from Example 1 was dosed into a suitable mixing vessel equipped with heating, cooling and mixing equipment. To 1 mole of hexamethylol melamine 30 moles of methanol were added, the pH was set to 1.5-1.9 with nitric acid and it was etherified at 45°C for 1.5 hours. Then the reaction mixture was neutralized with a NaOH solution and the volatile components were vacuum-distilled off.

References:

Melamin Kemicna tovarna d.d. Kocevje EP1607391, 2005, A1 Location in patent:Page/Page column 8

FullText