反应详情

温度

140 °C

A flask containing N-[4-(4-morpholinylmethyl)phenyl]tetrahydro-2H-pyran-4-amine (0.34 g) is treated with diethyl ethoxymethylenemalonate (0.30 mL) and pyridine (0.20 mL). The flask is tightly capped and heated to 140° C. for 2 hours. The reaction is cooled to room temperature and azeotroped under reduced pressure with toluene (3×). The residue is dissolved in dichloromethane and washed with water, brine, dried and concentrated under reduced pressure. The residue is chromatographed on silica eluting with 2% to 6% methanol in dichloromethane. The product-containing fractions are evaporated to give 0.41 g of diethyl 2-{[4-(4-morpholinylmethyl)(tetrahydro-2H-pyran-4-yl)anilino]methylene}malonate as a tan oil.

1. customThe flask is tightly capped
2. temperatureThe reaction is cooled to room temperature
3. customazeotroped under reduced pressure with toluene (3×)
4. dissolutionThe residue is dissolved in dichloromethane
5. washwashed with water, brine
6. customdried
7. concentrationconcentrated under reduced pressure
8. customThe residue is chromatographed on silica eluting with 2% to 6% methanol in dichloromethane
9. customThe product-containing fractions are evaporated