反应详情

To a solution of 1-tert-butyl 4-ethyl 4-((1-trityl-1H-imidazol-4-yl)methyl)piperidine-1,4-dicarboxylate from step A (330 mg, 0.57 mmol) in 1:1:2 THF:MeOH:H2O (10 mL) was added LiOH (136 mg, 5.7 mmol). The mixture was refluxed until LCMS showed complete conversion to product, then concentrated under vacuum, dissolved in water (3 mL), neutralized to pH 5-6 with aq. NaHSO4, and extracted with ethyl acetate (3×10 mL). The combined organic phases were washed with brine, dried over Na2SO4, and concentrated under vacuum to give the title compound (273 mg, 86%). MS (ES+) [M+H]+=552.2.

1. temperatureThe mixture was refluxed until LCMS
2. concentrationconcentrated under vacuum
3. dissolutiondissolved in water (3 mL)
4. extractionextracted with ethyl acetate (3×10 mL)
5. washThe combined organic phases were washed with brine
6. dry with materialdried over Na2SO4
7. concentrationconcentrated under vacuum