HRID1614549
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
A suspension of 5-bromo-1,2-dihydro-2,2-dimethyl-6-(2-imidazolin-2-ylamino)-3-(4H)-quinoxalinone (150 mg, 0.45 mmol) and LiALH4 (17 mg, 0.45 mmol) in tetrahydrofuran (3 ml) is heated and maintained at a temperature of 50°-80° C. until the starting material is consumed. The mixture is cooled to 0° C., 2-3 drops of H2O is added and the mixture is filtered. The solution is concentrated in vacuo to yield a residue which is chromatographed on silica gel with CHCl3 : CH3OH saturated with NH3 (g) elution to produce the title compound.
WORKUP
后处理
- temperatureis heated
- temperaturemaintained at a temperature of 50°-80° C. until the starting material
- customis consumed
- addition2-3 drops of H2O is added
- filtrationthe mixture is filtered
- concentrationThe solution is concentrated in vacuo
- customto yield a residue which
- customis chromatographed on silica gel with CHCl3
- washCH3OH saturated with NH3 (g) elution