反応 #3299

反応方程式

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

3-methyl-4-methoxyaniline

→

6-(2,6-Dichlorophenyl)-2-(4-methoxy-3-methylphenylamino)-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one

溶媒

Ether

反応条件

後処理

1. 1
   温度was heated
2. 2
   温度The resulting solution was heated for 5 minutes
3. 3
   温度cooled to room temperature
4. 4
   ろ過The crystals that developed were filtered
5. 5
   洗浄washed with 2 mL of ether
6. 6
   その他The solid was purified
7. 7
   その他to remove dark colors by silica gel chromatography
8. 8
   洗浄eluting with chloroform
9. 9
   濃縮The ethyl acetate eluent was concentrated to 3 mL volume
10. 10
    温度On cooling
11. 11
    その他pure crystals of product separated

実験手順

A mixture of 0.113 g (0.29 mmol) of 6-(2,6-dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 39 and 0.40 g (2.90 mmol) of 3-methyl-4-methoxyaniline was heated, with stirring, in a 165° C. oil bath. The resulting solution was heated for 5 minutes and cooled to room temperature. Ether (1 mL) was added. The crystals that developed were filtered and washed with 2 mL of ether; wt 0.109 g. The solid was purified to remove dark colors by silica gel chromatography, eluting with chloroform and then ethyl acetate. The ethyl acetate eluent was concentrated to 3 mL volume. On cooling, pure crystals of product separated; wt 0.060 g; mp 218°-220° C.

出典