HRID644461
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 2-bromo-1-(5-chloro-2-hydroxyphenyl)ethanone (156.9 mg, 0.63 mmol), thiourea (47.9 mg, 0.63 mmol) and ethanol (3 mL) was refluxed for 2 hours. After the reaction mixture was cooled to room temperature, it was poured into saturated sodium hydrogen carbonate solution and extracted with ethyl acetate. After the ethyl acetate layer was washed with brine and dried over anhydrous sodium sulfate, the residue obtained by evaporation of the solvent under reduced pressure was purified by column chromatography on silica gel (n-hexane:ethyl acetate=2:1) to give the title compound (98.6 mg, 64.5%) as a light yellowish white powder.
WORKUP
后处理
- temperaturewas refluxed for 2 hours
- extractionextracted with ethyl acetate
- washAfter the ethyl acetate layer was washed with brine
- dry with materialdried over anhydrous sodium sulfate
- customthe residue obtained by evaporation of the solvent under reduced pressure
- customwas purified by column chromatography on silica gel (n-hexane:ethyl acetate=2:1)