反应详情

温度

0 °C

16G (0.39 g, 0.85 mmol) prepared in the previous step was dissolved in 3 mL of anhydrous DCM. TEA (0.36 mL, 2.54 mmol) was added and the mixture was chilled to 0° C. To this chilled mixture, acetic anhydride (0.08 mL, 0.85 mmol) was added slowly. After about 30 minutes, TLC and LC/MS showed no signs of 16G. At this point, the mixture was concentrated to give tert-butyl 4-(1-(1-acetylpiperidin-3-yl)-2-oxo-5-phenyl-2,3-dihydro-1H-imidazole-4-carbonyl)piperazine-1-carboxylate (16H) as an oil (0.42 g, quantitative yield). ESI-MS: m/z 498.4 (M+H)+.

1. concentrationAt this point, the mixture was concentrated