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 mixture of 5.51 g (0.019 mole) of 4-[bis(4-fluorophenyl)methyl]piperidine, 4.42 g (0.019 mole) of 1-(3-chloropropoxy)-3,5-dimethoxybenzene and potassium carbonate (5.53 g, 0.04 mole) was heated overnight at reflux in 350 ml of 1-butanol containing potassium iodide (0.3 g). The reaction mixture was stripped to dryness and the residue partitioned between chloroform-5% sodium hydroxide and chloroform-water. Removal of chloroform gave a brown oil. The oil was subjected to chromatography on a silica gel column using a gradient elution series of hexane-ethyl acetate and ethyl acetate-dimethoxyethane. After combining proper fractions eluted from the column and removing solvent, the residual oil was dried in vacuo overnight at 80° C. This produced 2.61 g (28.5%) of brown oil.
WORKUP
后处理
- temperaturewas heated overnight
- customthe residue partitioned between chloroform-5% sodium hydroxide and chloroform-water
- customRemoval of chloroform
- customgave a brown oil
- washeluted from the column
- customremoving solvent
- customthe residual oil was dried in vacuo overnight at 80° C