Reaktion #3543

Reaktionsgleichung

water

sodium hydride

2,6-dichlorophenylacetonitrile

4-amino-2-phenylamino-pyrimidine-5-carboxaldehyde

4-Amino-2-phenylamino-pyrimidine-5-carboxaldehyde

→

title compound

Ausbeute 68.4%

6-(2,6-Dichlorophenyl)-N2 -phenyl-pyrido[2,3-d]-pyrimidine-2,7-diamine

Ausbeute 68.4%

Lösungsmittel

2-ethoxyethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction was refluxed for 4 hours
2. 2
   Temperaturcooled
3. 3
   Extraktionextracted several times with dichloromethane
4. 4
   Waschenwashed with saturated sodium chloride
5. 5
   Trocknendried with magnesium sulfate
6. 6
   Einengenconcentrated in vacuo
7. 7
   WaschenThe residue was washed with diethyl ether

Vorschrift

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+.

Quelle