反应详情

温度

80 °C

To a stirred suspension of 2-amino-5-(3-oxo-morpholin-4-yl)-benzonitrile (114 mg; example 21B) in acetonitrile/DMF 9:1 (5 ml) were added triethylamine (0.22 ml), (1R,3S,4S)-3-[(5-chloro-thiophene-2-carbonyl)-amino]-4-hydroxy-cyclopentanecarboxylic acid (198 mg) and BOP-Cl (174 mg). The reaction mixture was stirred at 80° C. overnight, then cooled to r.t. and concentrated. The crude product was purified by column chromatography (silica gel; gradient: CH2Cl2→CH2Cl2/MeOH 9:1) to give 5-chloro-thiophene-2-carboxylic acid {(1S,2S,4R)-4-[2-cyano-4-(3-oxo-morpholin-4-yl)-phenylcarbamoyl]-2-hydroxy-cyclopentyl}-amide (6 mg). Off-white solid. MS: 489.0 ([M+H]+).

1. temperaturecooled to r.t.
2. concentrationconcentrated
3. customThe crude product was purified by column chromatography (silica gel; gradient: CH2Cl2→CH2Cl2/MeOH 9:1)