HRID1773535
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
CONDITIONS
反应条件
- 温度
- 170 °C
PROCEDURE
实验过程
A mixture of 5-chloro-2,4-dinitrotoluene (1.0 g), 4-(hydroxymethyl)phenylboronic acid (0.84 g), bis(triphenylphosphine)palladium(II) chloride (150 mg) and potassium carbonate (2.0 g) in a mixture of 1,4-dioxane and water (10/1, 11 mL) was heated at 170° C. in a microwave reactor for 10 minutes. The reaction mixture was then cooled and diluted with ethyl acetate. The organic layer was washed with water and brine, dried over anhydrous sodium sulfate, filtered and evaporated under reduced pressure. The crude residue was purified by flash chromatography (acetone/DCM, 3/97) to give 0.6 g of (5′-methyl-2′,4′-dinitro-biphenyl-4-yl)-methanol.
WORKUP
后处理
- temperatureThe reaction mixture was then cooled
- washThe organic layer was washed with water and brine
- dry with materialdried over anhydrous sodium sulfate
- filtrationfiltered
- customevaporated under reduced pressure
- customThe crude residue was purified by flash chromatography (acetone/DCM, 3/97)