Reaktion #327785

Reaktionsgleichung

EtOAc

Methyl 4-(4-fluoro-2-hydroxyphenylamino)-5-methylthieno[2,3-d]pyrimidine-6-carboxylate

1-(methylsulfonyl)pyrrolidin-3-yl methansulfonate

potassium carbonate

→

4-[4-Fluoro-2-(1-methanesulfonyl-pyrrolidin-3-yloxy)-phenylamino]-5-methyl-thieno[2,3-d]pyrimidine-6-carboxylic acid methyl ester

Lösungsmittel

water

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe temperature was increased at 80° C.
2. 2
   Temperaturheated for 6 h again
3. 3
   Temperaturto cool overnight
4. 4
   Waschensolid washed with EtOAc
5. 5
   Sonstigeair-dried under vacuum

Vorschrift

Methyl 4-(4-fluoro-2-hydroxyphenylamino)-5-methylthieno[2,3-d]pyrimidine-6-carboxylate (described in V.1) (1.0 g), 1-(methylsulfonyl)pyrrolidin-3-yl methansulfonate and potassium carbonate (664.0 mg) were combined in DMF (15.0 ml) and heated at 60° C. overnight. The temperature was increased at 80° C. and heated for 6 h again. The reaction mixture was allowed to cool overnight. The mixture was portioned between EtOAc and water. The suspension was fitlered, solid washed with EtOAc and air-dried under vacuum.

Quelle