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
455 mg (1.12 mmol) 1-[3-(4-Heptyloxyphenoxy)-2-hydroxypropyl]indole-5-carbonitrile are dissolved in 10 ml tert-butanol. Having added 1.10 g (22.4 mmol) pulverized, 88% potassium hydroxide, the batch is heated to 100° C. for 3 hours. After cooling the reaction solution, hydrolysis using 50 ml distilled water and neutralization with 1 N hydrochloric acid are carried out. The aqueous phase is extracted three times with ethyl acetate and the combined organic phases are washed once with water and then twice with saturated sodium chloride solution. Following drying on sodium sulfate, the solvent is removed on the rotary evaporator. The residue is purified on silica gel by means of column chromatography (flow agent: ethyl acetate), the product accruing as a solid.
WORKUP
后处理
- additionHaving added 1.10 g (22.4 mmol)
- temperatureAfter cooling
- customthe reaction solution, hydrolysis
- distillationdistilled water and neutralization with 1 N hydrochloric acid
- extractionThe aqueous phase is extracted three times with ethyl acetate
- washthe combined organic phases are washed once with water
- customFollowing drying on sodium sulfate
- customthe solvent is removed on the rotary evaporator
- customThe residue is purified on silica gel by means of column chromatography (flow agent: ethyl acetate)