Water → HCID 67243482, compound

Participants

Reaction Steps

A solution of Intermediate 1 (337 mg) obtained in Example 1, Step A in methanol (2.7 ml) and pyridine (2.7 ml) is added with a solution of 28% sodium methylate (847 mg) in methanol, and then with copper iodide (70 mg), and the mixture is stirred at 65° C. for 30 hours. The reaction mixture is cooled to room temperature, and added with water (30 ml) and ethyl acetate (30 ml), and the insoluble matters are removed by filtration through Celite. The organic layer of the filtrate is separated, and the aqueous layer is extracted 3 times with ethyl acetate (20 ml for each time). The combined organic layer is washed 3 times with saturated brine (30 ml for each time), and dried over anhydrous magnesium sulfate. The solvent is evaporated under reduced pressure, and the residue is purified by silica gel chromatography (chloroform:methanol=30:1) to obtain the title compound (98 mg (predictive yield)).

Provenance & Evidence