反应详情

A mixture of 3-acetyl-5-(methyl(propyl)carbamoyl)-benzoic acid (from step 3, 0.386 mmol), HATU (176 mg, 0.464 mmol) and Hunig's base (200 mg, 0.3 mL, 1.545 mmol) in DMF (4.0 mL) was stirred for 10 min and then tert-butyl 3-methoxybenzyl((2R,3S)-3-amino-4-(3,5-difluorophenyl)-2-hydroxybutyl)-carbamate (168 mg, 0.386 mmol) was added. The reaction mixture was stirred at room temperature overnight. The reaction mixture was diluted with ethyl acetate and washed with H2O 3 times. The organic layer was dried over sodium sulfate and concentrated under vacuum. The crude product was purified by reverse phase prep HPLC to give the title compound (100 mg): HPLC retention time: 2.185 min (method A). MS (ESI) (M+H)+ 682.32.

1. stirringThe reaction mixture was stirred at room temperature overnight
2. washwashed with H2O 3 times
3. dry with materialThe organic layer was dried over sodium sulfate
4. concentrationconcentrated under vacuum
5. customThe crude product was purified by reverse phase prep HPLC