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
- 60 °C
PROCEDURE
实验过程
To a stirred solution of 4-(4-chlorophenoxy)piperidine hydrochloride (100 mg, 0.40 mmol), 5-(tert-butyl)isophthalic acid (358 mg, 1.61 mmol), and N,N-diisopropylethylamine (0.28 mL, 1.61 mmol) in N,N-dimethylformamide (3 mL) was add HBTU (183 mg, 0.48 mmol) at room temperature. After stirring at 60° C. for 2 hours, the mixture was poured into water (5 mL). This was extracted with ethyl acetate (5 mL) and washed with water (5 mL). The organic layer was dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica-gel column chromatography (eluting with dichloromethane/methanol=7:1) to give 121 mg (72% yield) of the title compound as a white solid.
WORKUP
后处理
- extractionThis was extracted with ethyl acetate (5 mL)
- washwashed with water (5 mL)
- dry with materialThe organic layer was dried over sodium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica-gel column chromatography (eluting with dichloromethane/methanol=7:1)