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
In 8 ml of dichloromethane were dissolved 66 mg of 4-(4-octyloxyphenyl)benzoyl chloride and 36 mg of (1R,2S)-1-cyano-2-hexyl-1-(4-hydroxyphenyl)cyclopropane as obtained in Example 11. Thereto was added 0.5 ml of pyridine. The resulting mixture was stirred for 8 hours with refluxing, and then cooled. Thereafter, 50 ml of ether was added to the reaction mixture, and the resulting mixture was washed with diluted hydrochloric acid, water, and saturated sodium chloride aqueous solution, and then dried over anhydrous sodium sulfate. The solvent was removed by evaporation, and the residue was separated and purified by silica gel column chromatography (solvent: hexane/ethyl acetate=5/1). Thus, 30 mg of the desired compound was obtained as colorless crystals.
WORKUP
后处理
- customas obtained in Example 11
- temperaturewith refluxing
- temperaturecooled
- washthe resulting mixture was washed with diluted hydrochloric acid, water, and saturated sodium chloride aqueous solution
- dry with materialdried over anhydrous sodium sulfate
- customThe solvent was removed by evaporation
- customthe residue was separated
- custompurified by silica gel column chromatography (solvent: hexane/ethyl acetate=5/1)