HRID1418785
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
- 0 °C
PROCEDURE
实验过程
19 g of vanadylacetylacetonate in solution of 50 ml of methylene chloride were cooled to 0° C. and 3.5 ml of terbutyl hydroperoxide in a toluene solution (3 M/l) were added over 30 minutes. The mixture was stirred for 20 minutes at 0° C. and 2.63 g of the product of Stage D in solution in 10 ml of methylene chloride were added. The reaction mixture was stirred for 3 hours at ambient temperature and 30 ml of water were added. The organic phase was separated and the solvent was eliminated under reduced pressure. The residue was chromatographed on silica (eluant: methylene chloride--acetone 8-2) to obtain 21.8 g of the expected product with a Rf=0.35 (CH2Cl2 --acetone 8-2).
WORKUP
后处理
- stirringThe reaction mixture was stirred for 3 hours at ambient temperature
- customThe organic phase was separated
- customThe residue was chromatographed on silica (eluant: methylene chloride--acetone 8-2)