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
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
2M aqueous sodium hydroxide solution (25 mL) was added to a solution of ethyl 6-(1-((6-cyclopropyl-3-ethoxy-2,4′-difluorobiphenyl-4-yl)methyl)piperidin-4-yl)-5-oxo-2-propyl-5,6,7,8-tetrahydro-1,6-naphthyridine-3-carboxylate (7.98 g) in ethanol (65 mL) at room temperature. The mixture was stirred at 80° C. under nitrogen atmosphere for 2 hours and concentrated in vacuo. The residue was dissolved in water. The solution was adjusted to neutral with 2M hydrochloric acid to give colorless crystals. After filtration, the crystals was dissolved in ethanol. The solution was filtrated and the filtrate was concentrated in vacuo. The residue was crystallized from ethyl acetate-hexane to give a colorless solid. The solid was recrystallized from ethanol-hexane to give the title compound (7.16 g).
WORKUP
后处理
- concentrationconcentrated in vacuo
- dissolutionThe residue was dissolved in water
- customto give colorless crystals
- filtrationAfter filtration
- dissolutionthe crystals was dissolved in ethanol
- filtrationThe solution was filtrated
- concentrationthe filtrate was concentrated in vacuo
- customThe residue was crystallized from ethyl acetate-hexane
- customto give a colorless solid
- customThe solid was recrystallized from ethanol-hexane