Synthesis
General procedure for the synthesis of n-butylthiophosphoric triamine from the compound (CAS: 6141-81-7): first, ammonia was passed through cold hydrazine and externally observed until liquid ammonia was formed. A cooling device was started in a four-necked flask equipped with a stirrer to maintain the reaction temperature at -45°C. Subsequently, 12.75 g of liquid ammonia was added to the flask and the pre-cooled reaction solution was added dropwise stepwise. The dropwise addition process was controlled to be completed within 1.5 hours. Samples were taken during the reaction and when the content of N-butylamino thiophosphoryl dichloride decreased to 2% of the total mass, the reaction temperature was raised to 25°C. The reaction was continued until the substitution reaction was completed, with a total reaction time of 2 h 5 min. At the end of the reaction, the product was filtered, washed and vaporized, and finally recrystallized from n-hexane to obtain N-n-butylaminophosphorothioic acid triamine with a purity of 98.7% and a yield of 95.1%.
References
[1] Patent: CN105399767, 2016, A. Location in patent: Paragraph 0045; 0047
[2] Patent: US2011/196172, 2011, A1. Location in patent: Page/Page column 4
[3] Chemische Berichte, 1956, vol. 89, p. 1768,1770
[4] Patent: US2011/28761, 2011, A1. Location in patent: Page/Page column 4
[5] Patent: CN105440073, 2016, A. Location in patent: Paragraph 0038; 0041
