تفاعل #3310

معادلة التفاعل

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

المذيبات

Water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas heated
2. 2
   درجة الحرارةThe resulting solution was heated for 10 minutes
3. 3
   درجة الحرارةcooled to room temperature
4. 4
   أخرىto precipitate a gum
5. 5
   أخرىThe mixture was decanted
6. 6
   أخرىthe remaining gum was triturated with 5 mL of water
7. 7
   ترشيحThe brown solid that developed was filtered
8. 8
   غسيلwashed well with water
9. 9
   أخرىdried
10. 10
    أخرىPurification
11. 11
    غسيلeluting with chloroform
12. 12
    أخرىwith ethyl acetate to obtain the fraction
13. 13
    workup.ADDITIONcontaining pure product
14. 14
    تركيزThe eluent was concentrated to 2 mL volume
15. 15
    أخرىThe crystals that separated on inducement
16. 16
    ترشيحwere filtered
17. 17
    غسيلwashed with 0.2 mL of ethyl acetate

الإجراء التجريبي

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.

المصدر