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N6-Methyl-2-methylthioadenosine synthesis

5synthesis methods
-

Yield:13406-51-4 52%

Reaction Conditions:

with potassium tert-butylate;palladium diacetate;triphenylphosphine;potassium thioacetate in dimethyl sulfoxide at 120;Inert atmosphere;

Steps:

39 Example 39

Under a nitrogen atmosphere,The substrate nucleoside derivative 1dd (0.1 mmol, 33.0 mg) was added to a 25 mL test tube reactor, KSAc(0.3mmol,34.2mg),DMC(0.5mmol,45mg),Pd(OAc)2(0.01mmol,2.3mg),PPh3 (0.02mmol,5.9mg),tBuOK(0.3mmol,34.6mg),and DMSO(1.5mL). The reaction was heated to 120 ° C to carry out the reaction. After the TLC detection reaction was completed,The system was cooled to room temperature.The reaction was quenched with saturated aqueous ammonium chloride,And extracted with ethyl acetate (3 * 10 mL)The column was purified by column chromatography to give the product 3d 18.3 mg (52%).

References:

CN106866327,2017,A Location in patent:Paragraph 0155; 0156; 0157