HRID1647170

反应详情

EQUATION

反应方程式

HRID 1647170 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customwas destroyed with addition of sodium thiosulphate (1 g)
  2. customThe organic phase was separated
  3. extractionthe aqueous phase was extracted with methylene chloride (3×50 ml)
  4. concentrationThe collected organic phases were concentrated under reduced pressure
  5. customchromatographed on silica (CH2Cl2 /MeOH, 90:10)