HRID1084469
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
- 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
- temperatureis heated for 24 hours
- temperaturecooled
- customchromatographed over silica gel
- extractionUsing cyclohexane as eluant, dichlorbenzene is first extracted
- customthe crude product is chromatographed with CH2Cl2
- customThe pre-purified product is chromatographed once more
- customthe solvent is removed by evaporation