HRID1647170
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
PROCEDURE
实验过程
To the methylene chloride solution of 2-methyl-3,4-methylenedioxypyridine from example I 21 sodium hydrogen carbonate (1M, 50 ml) and MCPBA (4 g, 70%) were added. The mixture was stirred at ambient temperature for 15 min whereupon the excess of MCPBA was destroyed with addition of sodium thiosulphate (1 g). The organic phase was separated and the aqueous phase was extracted with methylene chloride (3×50 ml). The collected organic phases were concentrated under reduced pressure and chromatographed on silica (CH2Cl2 /MeOH, 90:10). Yield: 120 mg (7,8%) of the title compound.
WORKUP
后处理
- customwas destroyed with addition of sodium thiosulphate (1 g)
- customThe organic phase was separated
- extractionthe aqueous phase was extracted with methylene chloride (3×50 ml)
- concentrationThe collected organic phases were concentrated under reduced pressure
- customchromatographed on silica (CH2Cl2 /MeOH, 90:10)