Reaktion #3302

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

3,4-dimethoxyaniline

→

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

Lösungsmittel

water

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe dark blue solution was cooled
2. 2
   Sonstigeto precipitate a solid
3. 3
   FiltrationThe solid was filtered
4. 4
   Waschenwashed well with water
5. 5
   Sonstigedried
6. 6
   SonstigePurification
7. 7
   Filtrationwas effected by filtration of an ethyl acetate (25 mL) solution through a layer of silica gel
8. 8
   Waschenwashing the silica gel with ethyl acetate
9. 9
   EinengenThe filtrate was concentrated to 3 mL volume
10. 10
    SonstigeThe crystals that separated on inducement
11. 11
    Filtrationwere filtered
12. 12
    Waschenwashed with 1 mL of ethyl acetate

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 (3.30 mmol) of 3,4-dimethoxyaniline was heated in a 160° C. oil bath for 5 minutes. The dark blue solution was cooled and dissolved in 2 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 0.200 g. Purification was effected by filtration of an ethyl acetate (25 mL) solution through a layer of silica gel and washing the silica gel with ethyl acetate. The filtrate was concentrated to 3 mL volume. The crystals that separated on inducement were filtered and washed with 1 mL of ethyl acetate and then 1 mL of ether; wt 0.116 g; mp 221°-223° C.

Quelle