HRID403954
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
Methyl 4-bromo-2-(bromomethyl)benzoate (650 mg, 2.12 mmol) and D-valine methyl ester hydrochloride (527 mg, 3.15 mmol) was taken in toluene (6.5 mL) and to this reaction mixture, triethyl amine (428 mg, 4.24 mmol) was added and refluxed for about 16 h. After completion of the reaction, the reaction mixture was diluted with ethyl acetate and washed with water and brine, dried over anhydrous sodium sulfate and concentrated to obtain an oil, which was purified by column chromatography (silica gel, 30% ethyl acetate in petroleum ether) to obtain the title compound.
WORKUP
后处理
- additionwas added
- temperaturerefluxed for about 16 h
- customAfter completion of the reaction
- washwashed with water and brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated
- customto obtain an oil, which
- customwas purified by column chromatography (silica gel, 30% ethyl acetate in petroleum ether)