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ASISCHEM W27133 synthesis

3synthesis methods
-

Yield:36881-76-2 90.7%

Reaction Conditions:

with caesium carbonate in N,N-dimethyl-formamide at 20; for 4 h;

Steps:

1

20.4 g of compound 2 was dissolved in 200 mL of DMF, 31.9 g of cesium carbonate and 13.9 g of methyl iodide were added. The reaction system was stirred at room temperature for 4 h, TLC followed the reaction. After completion of the reaction, the reaction system was added to 300 mL of ice water and the aqueous phase was extracted twice with 300 mL of ethyl acetate. The organic phases were combined, washed with 200 mL of water and saturated brine, and dried over anhydrous magnesium sulfate. After steaming the dry solvent, the residue was subjected to silica gel column chromatography (petroleum ether: ethyl acetate = 9: 1) to give 19.6 g of a white solid 3. Yield 90.7%. Melting point 55~56 °C .

References:

CN104447614,2017,B Location in patent:Paragraph 0009; 0015; 0017