反応 #3309

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

4-aminophenylacetic acid, methyl ester

acetic acid

→

{4-[6-(2,6-Dichlorophenyl)-8-methyl-7-oxo-7,8-dihydro-pyrido[2,3-d]pyrimidin-2-ylamino]phenyl}-acetic acid, methyl ester

溶媒

Water

反応条件

後処理

1. 1
   温度was heated in a 160° C. to 165° C. oil bath
2. 2
   温度The resulting solution was heated for 10 minutes
3. 3
   workup.DISSOLUTIONto dissolve
4. 4
   その他to precipitate a gum
5. 5
   その他The mixture was decanted
6. 6
   workup.DISSOLUTIONthe remaining gum was dissolved in 20 mL of chloroform
7. 7
   洗浄The chloroform solution was washed with 25 mL of water
8. 8
   乾燥dried (magnesium sulfate)
9. 9
   ろ過filtered
10. 10
    濃縮concentrated
11. 11
    その他Purification
12. 12
    洗浄eluting with chloroform
13. 13
    その他with 50% hexane/ethyl acetate to obtain the fraction
14. 14
    workup.ADDITIONcontaining pure product
15. 15
    濃縮The eluent was concentrated to dryness
16. 16
    その他to obtain a solid

実験手順

A mixture of 0.226 g (0.58 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 (2.80 mmol) of 4-aminophenylacetic acid, methyl ester base was heated in a 160° C. to 165° C. oil bath. The resulting solution was heated for 10 minutes and cooled to room temperature. The solution was treated with 1 mL of glacial acetic acid to dissolve. Water (10 mL) was added to precipitate a gum. The mixture was decanted, and the remaining gum was dissolved in 20 mL of chloroform. The chloroform solution was washed with 25 mL of water, dried (magnesium sulfate), filtered, and concentrated. Purification was effected by silica gel chromatography eluting with chloroform and then with 50% hexane/ethyl acetate to obtain the fraction containing pure product. The eluent was concentrated to dryness to obtain a solid; wt 0.141 g.

出典