Reaktion #357887

Reaktionsgleichung

4-amino-2-methylsulfanyl-pyrimidine-5-carbaldehyde

(3-amino-2,6-dichloro-phenyl)-acetonitrile

K2CO3

→

title intermediate

Ausbeute 80.0%

6-(3-Amino-2,6-dichloro-phenyl)-2-methylsulfanyl-pyrido[2,3-d]pyrimidin-7-ylamine

Ausbeute 80.0%

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe solution is cooled to room temperature
2. 2
   Sonstigethe solid is removed
3. 3
   Filtrationby filter paper
4. 4
   Einengenconcentrated
5. 5
   Sonstigeto give crude product
6. 6
   SonstigeFlash silica gel column purification
7. 7
   Wascheneluting with CH2Cl2 (100%) gradient to CH2Cl2/MeOH (2N NH3) (100/7%)

Vorschrift

A mixture of 4-amino-2-methylsulfanyl-pyrimidine-5-carbaldehyde (2.0 g, 11.82 mmol), (3-amino-2,6-dichloro-phenyl)-acetonitrile (2.85 g, 14.18 mmol) and K2CO3 (4.9 g, 35.49 mmol) in DMF (20 mL) is heated to 110° C. for 30 hours. The solution is cooled to room temperature and the solid is removed by filter paper and concentrated to give crude product. Flash silica gel column purification, eluting with CH2Cl2 (100%) gradient to CH2Cl2/MeOH (2N NH3) (100/7%), gives the title intermediate as a solid (3.31 g, 80.0%).

Quelle