HRID460533
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
200 mg of 6-(3-phenylamino-4-aminophenyl)oxyhexanoic acid methyl ester was mixed with 0.19 ml of tetraethylorthocarbonate and 40 μl of acetic acid, and the mixture was heated for 4 hours to 80° C. After cooling, it was mixed with 1N sodium hydroxide solution, extracted three times with ethyl acetate, the combined organic phases were washed with saturated sodium chloride solution, dried on sodium sulfate and concentrated by evaporation in a vacuum. The residue was purified by column chromatography on silica gel. 124 mg was obtained.
WORKUP
后处理
- temperaturethe mixture was heated for 4 hours to 80° C
- temperatureAfter cooling
- extractionextracted three times with ethyl acetate
- washthe combined organic phases were washed with saturated sodium chloride solution
- customdried on sodium sulfate
- concentrationconcentrated by evaporation in a vacuum
- customThe residue was purified by column chromatography on silica gel
- custom124 mg was obtained