HRID522925
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
- 120 °C
PROCEDURE
实验过程
To a solution of 3-(1,3-dioxoisoindolin-2-yl)propyl 4-methylbenzenesulfonate (3 g, 8.35 mmol) in DMF (25 mL, 3 mL/mmol) was added potassium carbonate (1.8 g, 12.5 mmol) and 4-trifluoromethoxyphenol (1.5 g, 8.35 mmol) and the reaction was heated at 120° C. for 2 h. The reaction mixture was concentrated under reduced pressure and extracted with EtOAc (2×60 mL). The organic extracts were washed with brine, dried over sodium sulfate and concentrated under reduced pressure. Purification by silica gel column chromatography provided 2-(3-(4-(trifluoromethoxy)phenoxy) propyl) isoindoline-1,3-dione (1 g, 33%) as a solid. Observed mass (M+1): 366.0.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated under reduced pressure
- extractionextracted with EtOAc (2×60 mL)
- washThe organic extracts were washed with brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated under reduced pressure
- customPurification by silica gel column chromatography