HRID1773536
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 solution of (5′-methyl-2′,4′-dinitro-biphenyl-4-yl)-methanol (0.6 g) in N,N-dimethylacetamide dimethylacetal (5 mL) was heated at 100° C. for 2 hour. The reaction mixture was then cooled, diluted with ethyl acetate, washed with a diluted aqueous solution of hydrochloric acid, 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 afford 1-(4′-hydroxymethyl-4,6-dinitro-biphenyl-3-yl)-propan-2-one.
WORKUP
后处理
- temperatureThe reaction mixture was then cooled
- washwashed with a diluted aqueous solution of hydrochloric acid, 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)