反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of (S)-methyl 2-(5-(4-(allyloxy)-4-methylpiperidin-1-yl)-2-(4′-fluoro-2′-((S)-pent-4-en-2-yloxy)-[1,1′-biphenyl]-3-yl)-7-methylimidazo[1,2-a]pyridin-6-yl)-2-(tert-butoxy)acetate (0.21 g, 0.307 mmol, 1 equiv) and TsOH monohydrate (58 mg, 0.307 mmol, 1 equiv) in DCE (300 mL) was heated to 80° C. The Hoveyda Grubbs 2nd generation catalyst (19 mg, 0.031 mmol, 0.1 equiv) was added. The pale green brown solution was stirred for 2 h. Upon cooling to ambient temperature, the reaction was washed with saturated aqueous NaHCO3, dried (Na2SO4), and concentrated in vacuo. The crude product was purified by flash column chromatography (0-100% EtOAc [2% TEA]/hexane) to provide the product (0.20 g, 99%) as a yellow glass. LCMS (ESI, M+1): 656.25.
WORKUP
后处理
- washthe reaction was washed with saturated aqueous NaHCO3
- dry with materialdried (Na2SO4)
- concentrationconcentrated in vacuo
- customThe crude product was purified by flash column chromatography (0-100% EtOAc [2% TEA]/hexane)