反应详情

温度

80 °C

A suspension of Intermediate 26 (0.20 g), and potassium carbonate (0.31 g) in 1,3-dimethyl-2-imidazolidinone (3 ml, Tokyo Kasei Kogyo) is added with 25% aqueous ammonia (2 ml), and the mixture is stirred at 80° C. for 24 hours in a sealed tube. The reaction mixture is added with saturated brine (30 ml), and extracted 3 times with chloroform (30 ml for each time). The combined organic layer is washed twice with saturated brine (50 ml for each time), and dried over anhydrous magnesium sulfate. The solvent is evaporated under reduced pressure, and the residue is purified by silica gel chromatography (chloroform:methanol=9:1) to obtain the title compound (64.4 mg (predictive yield)).

1. extractionextracted 3 times with chloroform (30 ml for each time)
2. washThe combined organic layer is washed twice with saturated brine (50 ml for each time), and
3. dry with materialdried over anhydrous magnesium sulfate
4. customThe solvent is evaporated under reduced pressure
5. customthe residue is purified by silica gel chromatography (chloroform:methanol=9:1)