Reaktion #3301

Reaktionsgleichung

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

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

4-ethoxyaniline

→

6-(2,6-Dichlorophenyl)-2-(4-ethoxyphenylamino)-8-ethyl-8H-pyrido[2,3-d]pyrimidin-7-one

Lösungsmittel

water

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigewas fused in a 160° C.
2. 2
   Sonstigefor 10 minutes
3. 3
   TemperaturThe dark violet melt was cooled
4. 4
   Sonstigeto precipitate a solid
5. 5
   FiltrationThe solid was filtered
6. 6
   Waschenwashed well with water
7. 7
   Sonstigedried
8. 8
   SonstigePurification
9. 9
   Filtrationwas effected by filtration of an ethyl acetate solution through a layer of silica gel
10. 10
    Waschenwashing the silica gel with ethyl acetate
11. 11
    EinengenThe filtrate was concentrated to 2 mL volume and 2 mL of petroleum ether
12. 12
    workup.ADDITIONwas added
13. 13
    SonstigeThe crystals that separated on inducement
14. 14
    Filtrationwere filtered
15. 15
    Waschenwashed with ether

Vorschrift

A mixture of 0.150 g (0.38 mmol) of 6-(2,6-dichlorophenyl)-8-ethyl-2-methanesulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 68 and 0.500 g (3.60 mmol) of 4-ethoxyaniline was fused in a 160° C. oil bath for 10 minutes. The dark violet melt was cooled and dissolved in 1 mL of warm glacial acetic acid. This solution was diluted to 10 mL volume with water to precipitate a solid. The solid was filtered, washed well with water, and dried; wt 0.140 g. Purification was effected by filtration of an ethyl acetate solution through a layer of silica gel and washing the silica gel with ethyl acetate. The filtrate was concentrated to 2 mL volume and 2 mL of petroleum ether was added. The crystals that separated on inducement were filtered and washed with ether; wt 0.094 g; mp 192°-194° C.

Quelle