Benzoic Acid → HCID 66852565, compound

Participants

Reaction Steps

The compound of Example 18 (292 mg), benzoic acid (61 mg) and triethylamine (0.2 mL) was dissolved in 3 mL of DMF, to the above solution, 80 mg of HOBt was added under stirring at ice temperature. After stirring the mixture at the same temperature for 15 minutes, thereto 115 mg of WSC was added, and the mixture was stirred at room temperature overnight. The reaction solution was evaporated to dryness under reduced pressure, and ice-water was added to the resulting residue, and the mixture was extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate, and then concentrated to dryness under reduced pressure. The residue was purified by chromatography on silica gel (methylene chloride-methanol-triethylamine=300:10:1) to give 261 mg of N-(4-{6-amino-2-[6-(4-benzoylpiperazin-1-ylmethyl)pyridin-2-ylmethylsulfanyl]-5-cyanopyrimidin-4-yl}phenyl)acetamide as a white powder.

Provenance & Evidence