HRID444450

反应详情

EQUATION

反应方程式

HRID 444450 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.6 g of a sodium hydride suspension (55%) are added in portions, at 0°-5°, to 15.7 g of 3-(2,3-epoxypropoxy)-2-nitro-pyridine and 9.0 g of benzyl alcohol dissolved in 150 ml of 1,2-dimethoxyethane, with stirring and cooling, and the mixture is stirred for a further 3 hours at 0°-5° and for 2 hours at 20°-25°. The reaction mixture is evaporated, the residue is dissolved in ethyl acetate, the solution is washed with water and the ethyl acetate solution is evaporated. The residue (20 g) is chromatographed on 400 g of silica gel and eluted with toluene (250 ml fractions). 2-Benzyloxy-3-(2,3-epoxypropoxy)-pyridine is obtained in the form of an oil from fractions 28-36.

WORKUP

后处理

  1. temperaturecooling
  2. stirringthe mixture is stirred for a further 3 hours at 0°-5° and for 2 hours at 20°-25°
  3. customThe reaction mixture is evaporated
  4. dissolutionthe residue is dissolved in ethyl acetate
  5. washthe solution is washed with water
  6. customthe ethyl acetate solution is evaporated
  7. customThe residue (20 g) is chromatographed on 400 g of silica gel
  8. washeluted with toluene (250 ml fractions)