HRID1084469

反应详情

EQUATION

反应方程式

HRID 1084469 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

A mixture of 0.27 g (0.0012 mol) of 4-benzylthio-2-oxo-2H-pyrane, 0.25 g (0.0012 mol) of 1,4-anthraquinone and 0.10 g (0.0012 mol) of MnO2 in 5 ml of dichlorobenzene is heated for 24 hours under reflux (180° C.), then cooled and chromatographed over silica gel. Using cyclohexane as eluant, dichlorbenzene is first extracted, then the crude product is chromatographed with CH2Cl2. The pre-purified product is chromatographed once more, using CH2Cl2 as eluant, and the solvent is removed by evaporation. Yield: 0.09 g (20%). Melting point: 200°-203° C.

WORKUP

后处理

  1. temperatureis heated for 24 hours
  2. temperaturecooled
  3. customchromatographed over silica gel
  4. extractionUsing cyclohexane as eluant, dichlorbenzene is first extracted
  5. customthe crude product is chromatographed with CH2Cl2
  6. customThe pre-purified product is chromatographed once more
  7. customthe solvent is removed by evaporation