HRID1893490
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A solution of 8-(benzylamino)-7-(trifluoromethyl)imidazo[1,2-a]quinoxalin-4(5H)-one (72 mg; 0.2 mmol; 1 eq) and N,N′-dimethylaniline (0.2 ml) in phosphoryl chloride (2 ml) is stirred at 135° C. under argon for 2 h. Concentration, partition (ice water/ethyl acetate), extraction of the aqueous phase (ethyl acetate), reunion of the organic phases, drying (magnesium sulfate), concentration and purification by prep CCM on silicagel (dichloromethane/methanol 90:10) affords the title product (35 mg; 0.093 mmol; 47%) as a yellow solid.
WORKUP
后处理
- concentrationConcentration
- custompartition
- extraction(ice water/ethyl acetate), extraction of the aqueous phase (ethyl acetate), reunion of the organic phases
- customdrying
- concentration(magnesium sulfate), concentration and purification by prep CCM on silicagel (dichloromethane/methanol 90:10)