Ethylenediamine → N~2~,N~2'~-(Ethane-1,2-diyl)di(1,3,5-triazinane-2,4,6-triimine)

29.1 g of 2,4-diamino-6-chloro-s-triazine was added to 300 ml of water to obtain a slurry. Then 6 g of ethylenediamine was added thereto, and the mixture was stirred for 15 minutes. Then, 16 g of a 25 wt% sodium hydroxide aqueous solution was added thereto, and the mixture was refluxed under heating for two hours. At that time, about 3 g of a 25 wt% sodium hydroxide aqueous solution was further gradually added over a period of two hours to maintain the reaction solution in a weakly alkaline state. After completion of the reaction, the reaction mixture was left to cool, whereupon the crystals were collected by filtration and washed with water to obtain 25.3 g of ethylenebismelamine. Then, 5.9 g of ethylenebismelamine and 17 g of formaline were mixed, and mixture was subjected to a heating reaction at 90° C. for 4 hours while maintaining the mixture at pH 9 to 10 with an aqueous sodium hydroxide solution. Then, the formed methylol product was taken out, and 30 ml of methanol was added thereto. The mixture was adjusted to pH 4 with hydrochloric acid. After the solution became uniform, it was heated for 5 minutes and neutralized. Then, methanol was distilled off to obtain 3.2 g of methoxymethylated ethylenebismelamine. The product was analyzed by IR and NMR and was found to be a mixture containing octamethoxymethylethylenebismelamine as the main component.

1. customto obtain a slurry
2. temperaturethe mixture was refluxed
3. temperatureunder heating for two hours
4. temperatureto maintain the reaction solution in a weakly alkaline state
5. customAfter completion of the reaction
6. waitthe reaction mixture was left
7. temperatureto cool, whereupon the crystals
8. filtrationwere collected by filtration
9. washwashed with water

ORD record

ord-ef596feca9b14529a35f4f472157e6ed

Source dataset

uspto-grants-1994_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05292614