ChemicalBook CAS DataBase List GS-441524

GS-441524 synthesis

7synthesis methods

Product Name:GS-441524
CAS Number:1191237-69-0
Molecular formula:C12H13N5O4
Molecular Weight:291.26

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1191237-69-0
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Yield:1191237-69-0 95%

Reaction Conditions:

with boron trichloride in dichloromethane at 5;

Steps:

1

(1) Material preparation: Dissolve about 200g of raw materials in dichloromethane to prepare 0.5mmol/mL raw material liquid, and place it in the raw material liquid bottle;1.0mmol/mL boron trichloride dichloromethane solution (about 1200mL) is directly used as the auxiliary material liquid and placed in the auxiliary material liquid bottle;Connect the raw material liquid bottle to the metering pump A;Connect the auxiliary material liquid bottle to the metering pump B;(2) Reaction temperature parameter setting: start the circulating liquid cooling system, make the mixer and the main reaction pipeline at about 5 degrees of the set temperature;(3) Material flow rate parameter setting: the flow rate parameter of metering pump A is set to 25mL/min (12.5mmol/min); the flow rate parameter of metering pump B is set to 37.5mL/min (37.5mmol/min);(4) Continuous flow reaction system operation: start two pump systems at the same time, metering pump A and metering pump B respectively send the raw material liquid and auxiliary material liquid into the mixer at their respective set flow rates; the two feed liquids are mixed in the pre-cooling mixer (Holding liquid retention time is about 12 seconds), and then enters the pre-cooling main reaction pipeline (Holding liquid retention time is about 50 seconds);(5) Quenching process: the reaction liquid flows out into an aqueous sodium hydroxide solution (120g sodium hydroxide, dissolved in 1.8kg water) for quenching;(6) Post-treatment process: filtering, adding the obtained crude product to 150 g of methanol, beating and filtering to obtain 98.5 g of the target product, with a yield of 95%, a purity of the high performance liquid phase of 99.4%, and a single impurity of less than 0.15%.

References:

CN112745324,2021,A Location in patent:Paragraph 0040-0048