反応 #3310

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

5-amino-2-methoxypyridine

→

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

溶媒

Water

反応条件

後処理

1. 1
   温度was heated
2. 2
   温度The resulting solution was heated for 10 minutes
3. 3
   温度cooled to room temperature
4. 4
   その他to precipitate a gum
5. 5
   その他The mixture was decanted
6. 6
   その他the remaining gum was triturated with 5 mL of water
7. 7
   ろ過The brown solid that developed was filtered
8. 8
   洗浄washed well with water
9. 9
   その他dried
10. 10
    その他Purification
11. 11
    洗浄eluting with chloroform
12. 12
    その他with ethyl acetate to obtain the fraction
13. 13
    workup.ADDITIONcontaining pure product
14. 14
    濃縮The eluent was concentrated to 2 mL volume
15. 15
    その他The crystals that separated on inducement
16. 16
    ろ過were filtered
17. 17
    洗浄washed with 0.2 mL of ethyl acetate

実験手順

A mixture of 0.155 g (0.40 mmol) of 6-(2,6-dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 39 and 0.50 g (4.00 mmol) of 5-amino-2-methoxypyridine was heated, with stirring, in a 160° C. oil bath. The resulting solution was heated for 10 minutes and cooled to room temperature. Water (10 mL) was added to precipitate a gum. The mixture was decanted, and the remaining gum was triturated with 5 mL of water. The brown solid that developed was filtered, washed well with water, and dried; wt 0.135 g. Purification was effected by silica gel chromatography eluting with chloroform and then with ethyl acetate to obtain the fraction containing pure product. The eluent was concentrated to 2 mL volume. The crystals that separated on inducement were filtered and washed with 0.2 mL of ethyl acetate and then 0.5 mL of ether; wt 0.045 g; mp 233°-235° C.

出典