反应详情

温度

0 °C

To a solution of (S)-4-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-5-oxo-5-((S)-6-phenethylcarbamoyl-tetrahydro-pyridazin-1-yl)-pentanoic acid (0.74 g, 1.5 mmol) and N-methylmorpholine (0.6 g, 6.0 mmol) in THF (20 mL) at 0° C., is added PCl5 (470 mg, 2.25 mmol) in one portion. After stirring at 0° C. for 3 hours, the reaction mixture is concentrated and purified by chromatography (CH2Cl2/MeOH:97/3) to yield (1S,9S)-9-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-6,10-dioxo-octahydro-pyridazino[1,2-a][1,2]diazepine-1-carboxylic acid phenethyl-amide (310 mg, 43.6%) as white solid. (NMR and MS data confirmed, U-3133-65).

1. concentrationthe reaction mixture is concentrated
2. custompurified by chromatography (CH2Cl2/MeOH:97/3)