HRID444450
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
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
- temperaturecooling
- stirringthe mixture is stirred for a further 3 hours at 0°-5° and for 2 hours at 20°-25°
- customThe reaction mixture is evaporated
- dissolutionthe residue is dissolved in ethyl acetate
- washthe solution is washed with water
- customthe ethyl acetate solution is evaporated
- customThe residue (20 g) is chromatographed on 400 g of silica gel
- washeluted with toluene (250 ml fractions)