Reaktion #3293

Reaktionsgleichung

6-(2,6-dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one

6-(2,6-Dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one

cyclohexylamine

→

2-Cyclohexylamino-6-(2,6-dichlorophenyl)-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe resulting solution was heated
2. 2
   Temperaturat reflux for 2 minutes
3. 3
   SonstigeMost of the excess amine was evaporated at reduced pressure
4. 4
   workup.DISSOLUTIONThe remaining gum was dissolved in 2 mL of ethyl acetate hot
5. 5
   workup.ADDITIONPetroleum ether (2 mL) was added
6. 6
   Sonstigethe crystals that separated from the cooled solution
7. 7
   Filtrationwere filtered
8. 8
   Waschenwashed with water
9. 9
   SonstigeRecrystallization from ethyl acetate
10. 10
    Sonstigegave pure crystalline product

Vorschrift

A mixture of 0.100 g (0.26 mmol) of 6-(2,6-dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 39 and 0.300 g (3.00 mmol) of cyclohexylamine was heated to the boiling point (134° C.). The resulting solution was heated at reflux for 2 minutes. Most of the excess amine was evaporated at reduced pressure. The remaining gum was dissolved in 2 mL of ethyl acetate hot. Petroleum ether (2 mL) was added, and the crystals that separated from the cooled solution were filtered and washed with water; wt 0.090 g. Recrystallization from ethyl acetate gave pure crystalline product; 0.048 g; mp 242°-244° C.

Quelle