Chloroform → HCID 46865142, compound

Participants

Reaction Conditions

Reaction Steps

Saturated sodium bicarbonate aqueous solution and chloroform were added to 141 mg of (S)—N4-(2-aminoethyl)-N2-[1-(4-fluorophenyl)ethyl]-N6-(pyrazin-2-yl)pyrimidine-2,4,6-triamine dihydrochloride (Example 76), and the mixture was subjected to extraction. The organic layer washed with brine, and dried over magnesium sulfate. The solvent was distilled off under reduced pressure, and then the obtained residue was dissolved in 3 ml of tetrahydrofuran, and 223 μl of diisopropylethylamine and 23 μl of acetyl chloride were added at 0° C., and the mixture was stirred at 0° C. for 30 minutes. The reaction solution was added with water and subjected to extraction with ethyl acetate. The organic layer washed with brine, and dried over magnesium sulfate. The solvent was distilled off under reduced pressure, and then the obtained residue was purified by silica gel column chromatography to obtain 95 mg of (S)—N-(2-{2-[1-(4-fluorophenyl)ethylamino]-6-(pyrazin-2-ylamino)pyrimidin-4-ylamino}ethyl)acetamide as white powder. The obtained compound was subjected to hydrochlorination using a conventional method to obtain 74 mg of the objective compound as pale yellow powder.

Provenance & Evidence