Adding a certain compound to certain chemical reactions, such as: 145783-15-9, 4,6-Dichloro-2-(propylthio)pyrimidin-5-amine, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, name: 4,6-Dichloro-2-(propylthio)pyrimidin-5-amine, blongs to pyrimidines compound. name: 4,6-Dichloro-2-(propylthio)pyrimidin-5-amine
3) Operation process(1) Add 18L of ethylene glycol and 9.335kg of SM1 to the 100L reactor.12kg SM2 and 16.529kg triethylamine,Stir and mix;(2) heating the reaction solution to 90 ~ 100 C, the reaction liquid solid dissolved, the color is a yellow clear solution; maintaining this temperature for 8 to 10 hours;(3) TLC detection, the developing agent is ethyl acetate: methanol = 1:1, the color developing agent is ninhydrin ethanol solution, and the color is baked at 150 C;Lower the reaction solution to below 50 C,The reaction solution is a dark brown clear solution;The reaction solution was poured into a 200 L reaction vessel containing 50 L of ethyl acetate and 50 L of water under stirring at room temperature;The 100 L reaction kettle was rinsed with 10 L of ethyl acetate and 10 L of purified water.The eluent was poured into a 200 L reaction kettle; stirred at room temperature for 30 minutes; the stirring was stopped, and the layer was allowed to stand.Divide the lower aqueous phase;(4) Add 60 L of purified water to the upper organic phase, stir at room temperature for 30 minutes; stop stirring, let stand for stratification, and separate the lower layer.water box;(5) Transfer the upper organic phase to a 500L reactor and heat to 60-70 C with stirring; in addition, 180 L of isooctane pre-Heat to 60 ~ 70 C, added to the reaction flask;(8) After adding, slowly cool down to room temperature with stirring and firstly cool to 35-45 C (solid precipitation temperature about 30-35 C).Slowly cool down to 20 ~ 30 C; keep stirring at 20 ~ 30 C for 1 hour, and then slowly reduce the temperature to 0 ~ 10 C;(8) stirring at 0 to 10 C for 2 hours;(9) Centrifugal filtration, the reaction kettle and filter cake are mixed with 12 L of ethyl acetate pre-cooled to 0-10 C and 36 L of isooctane.Rinsing(10) The filter cake is dried under vacuum at 45-55 C for 12 to 16 hours to obtain a white powder of Im-1, weighing 11 kg, yield80%.
The synthetic route of 145783-15-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Hebei Kaiwei Pharmaceutical Co., Ltd.; Pang Yuning; (23 pag.)CN108276417; (2018); A;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia