반응 #3292

반응 방정식

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

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

1-(4-aminobutyl)-4-methylpiperazine

→

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

용매

ether

반응 조건

후처리

1. 1
   온도was heated
2. 2
   workup.WAITAfter 2 hours
3. 3
   온도the solution was cooled to room temperature
4. 4
   세척The solution was washed with 4×5 mL of water
5. 5
   세척wash
6. 6
   건조The ether solution was dried over potassium carbonate
7. 7
   여과filtered
8. 8
   농축concentrated to ca. 2 mL volume
9. 9
   기타The crystals that separated on inducement
10. 10
    여과were filtered
11. 11
    세척washed with ether

실험 절차

A mixture of 0.152 g (0.43 mmol) of 6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfanyl-8-pyrido[2,3-d]pyrimidin-7-one of Example 37 and 0.50 g (2.90 mmol) of 1-(4-aminobutyl)-4-methylpiperazine was heated with stirring in a 170° C. oil bath. After 2 minutes, solution was complete. After 2 hours, the solution was cooled to room temperature, and the dark gum was dissolved in 25 mL of ether. The solution was washed with 4×5 mL of water. Most of the color went into the water wash. The ether solution was dried over potassium carbonate, filtered, and concentrated to ca. 2 mL volume. The crystals that separated on inducement were filtered and washed with ether; wt 0.063 g; mp 130°-132° C.;

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