SELEXIPAG interMediate synthesis

4synthesis methods

Product Name:SELEXIPAG interMediate
CAS Number:475086-75-0
Molecular formula:C23H27N3O
Molecular Weight:361.48

41270-66-0 Synthesis

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42042-71-7 Synthesis

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Yield:475086-75-0 96%

Reaction Conditions:

with tris-(o-tolyl)phosphine;Palladium⁽⁰⁾ bis(dibenzylideneacetone);sodium tertiary butoxide in 1,4-dioxane at 120; for 1.8 h;Reagent/catalyst;Temperature;Solvent;

Steps:

7 Example 7

In one embodiment of the preparation method of the sirepag intermediate of the present invention, the preparation method of the siriparg intermediate according to the present embodiment is: in a reaction bottle equipped with a reflux tube, a drying tube and a thermometer, adding 5- Chloro-2,3-diphenylpyrazine (30.0 g, 0.11 mol, 1.0 eq.), 4-(isopropylamino)-1-butanol (18.5 g, 0.14 mol, 1.25 eq.), 1, 4-Dioxane 150 mL, stir and dissolve, and then add Pd (dba)₂(2.4g, 4.2mmol), P(o-tolyl)₃(1.69 g, 8.3 mmol), sodium tert-butoxide (13.0 g, 0.135 mol), heated to 120° C., and incubated for 1.8 hours. The reaction was complete by TLC and the reaction was stopped.The mixture was cooled to room temperature and filtered. The filtrate was adjusted to pH 6.5-7.5 with 1N hydrochloric acid, extracted with ethyl acetate (150 mL x 2), washed with 150 mL of brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure with the residue being ethanol: The mixture was recrystallized with 300 mL of n-hexane = 1:15 mixed solvent and dried in an oven to obtain 39.0 g of a white solid. The yield was 96%, and the liquid purity was 97.1%.

References:

CN107652243,2018,A Location in patent:Paragraph 0038; 0041-0045; 0047; 0049-0051; 0053; 0055; 0058

42042-71-7 Synthesis

42042-71-7
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$6.00/250mg