HRID2235509
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a mixture of 1-(5-dipropylamino-2-methylphenyl)-3-mesitylthiourea (100 mg, 0.261 mmol) in carbon tetrachloride (10 ml) was added dropwise bromine (0.015 ml, 0.287 mmol) in carbon tetrachloride (5 ml) over 30 min. The mixture was refluxed for 18 h and diluted with water. The aqueous solution was extracted with dichloromethane. The extract was washed with water and brine and concentrated under vacuum. The residue was purified by chromatography eluting with 10% AcOEt in n-hexane to afford 39 mg of the title compound.
WORKUP
后处理
- temperatureThe mixture was refluxed for 18 h
- extractionThe aqueous solution was extracted with dichloromethane
- washThe extract was washed with water and brine
- concentrationconcentrated under vacuum
- customThe residue was purified by chromatography
- washeluting with 10% AcOEt in n-hexane