تفاعل #3306

معادلة التفاعل

6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one

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

1-(5-aminopentyl)-4-methylpiperazine

→

6-(2,6-Dichlorophenyl)-8-methyl-2-[5-(4-methylpiperazin-1-yl)-pentylamino]-8H-pyrido[2,3-d]pyrimidin-7-one

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas heated
2. 2
   workup.WAITAfter 0.5 hour
3. 3
   أخرىto precipitate a taffy-like gum
4. 4
   أخرىDecanted
5. 5
   أخرىtriturated gum again with 5 mL of water
6. 6
   أخرىDecanted
7. 7
   غسيلThe ether solution was washed with 2×50 mL of water
8. 8
   تجفيفdried (potassium carbonate)
9. 9
   تركيزconcentrated to 5 mL volume
10. 10
    workup.ADDITIONPetroleum ether was added to slight turbidity
11. 11
    أخرىThe crystals that separated on inducement
12. 12
    ترشيحwere filtered
13. 13
    غسيلwashed with 80% ether/petroleum ether

الإجراء التجريبي

A mixture of 0.165 g (0.47 mmol) of 6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 37 and 0.50 g (2.70 mmol) of 1-(5-aminopentyl)-4-methylpiperazine was heated with stirring in a 180° C. to 185° C. oil bath. After 2 minutes, solution was complete. After 0.5 hour, the solution was cooled to room temperature, and 5 mL of water was added to precipitate a taffy-like gum. Decanted and triturated gum again with 5 mL of water. Decanted and took up gum into 35 mL of ether. The ether solution was washed with 2×50 mL of water, dried (potassium carbonate), and concentrated to 5 mL volume. Petroleum ether was added to slight turbidity. The crystals that separated on inducement were filtered and washed with 80% ether/petroleum ether; wt 0.060 g; mp 110°-112° C.;

المصدر