反应详情

A solution of methyl 3-[({3-[(6-cyano-1H-benzimidazol-1-yl)methyl]-1-hydroxycyclohexaneyl}methyl)amino]-2,2-dimethylpropanoate (1.048 g, 2.63 mmol) and CDI (0.853 g, 5.26 mmol) in 1,4-dioxane (15 mL) was stirred at 100° C. for 1 day. The reaction was then concentrated and purified via silica gel chromatography (ISCO, 40 g silica gel column; solvent A=DCM; solvent B=MeOH (0.1M NH3); 0-5% B over 15 min; then 5% B over 5 min) to give methyl 3-{(5S,7S)-7-[(6-cyano-1H-benzimidazol-1-yl)methyl]-2-oxo-1-oxa-3-azaspiro[4.5]dec-3-yl}-2,2-dimethylpropanoate as a beige solid (1.06 g, 95% yield). MS (m/z) 425.2 (M+H+).

1. concentrationThe reaction was then concentrated
2. custompurified via silica gel chromatography (ISCO, 40 g silica gel column