HRID1460623

反应详情

EQUATION

反应方程式

HRID 1460623 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

12 g of the above chromene are dissolved in 400 ml of abs. dichloromethane, the obtained solution is mixed with anhydrous sodium bicarbonate and oxidized during 3 days with 31 mg of m-chloroperbenzoic acid. The slightly yellow suspension is partitioned between an aq. ammoniumhydroxide solution (5%) and dichlormethane, the organic phases are washed with water and dried over sodiumsulphate. The oil, obtained after concentration, is purified by flash-chromatography (silica gel/dichloromethane, hexane 2:3). Besides of educt, 2,2-diethyl-3,4-epoxy-3,4-dihydro-2H-1-benzopyran-6-carbonitrile is obtained as colorless oil.

WORKUP

后处理

  1. customThe slightly yellow suspension is partitioned between an aq. ammoniumhydroxide solution (5%) and dichlormethane
  2. washthe organic phases are washed with water
  3. dry with materialdried over sodiumsulphate
  4. customThe oil, obtained
  5. concentrationafter concentration
  6. customis purified by flash-chromatography (silica gel/dichloromethane, hexane 2:3)