HRID1773536

反应详情

EQUATION

反应方程式

HRID 1773536 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe reaction mixture was then cooled
  2. washwashed with a diluted aqueous solution of hydrochloric acid, water and brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. customevaporated under reduced pressure
  6. customThe crude residue was purified by flash chromatography (acetone/DCM, 3/97)