反应详情

To a solution of 0.022 g 60% sodium hydride suspension in 2.00 mL of 2-ethoxyethanol was added 0.46 g of 2,6-dichlorophenylacetonitrile and 0.50 g of 4-amino-2-phenylamino-pyrimidine-5-carboxaldehyde from Example 72. The reaction was refluxed for 4 hours, cooled, poured into water, and extracted several times with dichloromethane. The dichloromethane washes were combined, washed with saturated sodium chloride, dried with magnesium sulfate, and concentrated in vacuo. The residue was washed with diethyl ether to give 0.61 g of the title compound, CIMS (1% NH3 in CH4): 410=M+ +C2H5, 382=M+ +H, 381=M+.

1. temperatureThe reaction was refluxed for 4 hours
2. temperaturecooled
3. extractionextracted several times with dichloromethane
4. washwashed with saturated sodium chloride
5. dry with materialdried with magnesium sulfate
6. concentrationconcentrated in vacuo
7. washThe residue was washed with diethyl ether