反应详情

温度

160 °C

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 (2.70 mmol) of 3,4,5-trimethoxyaniline was heated in a 160° C. oil bath for 5 minutes. The dark solution was cooled and dissolved in 2 mL of warm glacial acetic acid. This solution was diluted to 15 mL volume with water to precipitate a violet solid. The solid was filtered, washed well with water, and dried; wt 0.140 g. Purification was effected by filtration of an ethyl acetate (30 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 1 mL of ether; wt 0.054 g; mp 275°-278° C.

1. temperatureThe dark solution was cooled
2. customto precipitate a violet solid
3. filtrationThe solid was filtered
4. washwashed well with water
5. customdried
6. customPurification
7. filtrationwas effected by filtration of an ethyl acetate (30 mL) solution through a layer of silica gel
8. washwashing the silica gel with ethyl acetate
9. concentrationThe filtrate was concentrated to 3 mL volume
10. customThe crystals that separated on inducement
11. filtrationwere filtered
12. washwashed with 1 mL of ethyl acetate and 1 mL of ether