4-(4-Methylpiperazin-1-yl)butan-1-amine → 2-aminopyrido[2,3-d]pyrimidin-7(8H)-one 32

HRID 3196

反応式

HRID 3196 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:20](=[O:21])[N:19]([CH3:22])[C:12]2[N:13]=[C:14](SC)[N:15]=[CH:16][C:11]=2[CH:10]=1.[NH2:23][CH2:24][CH2:25][CH2:26][CH2:27][N:28]1[CH2:33][CH2:32][N:31]([CH3:34])[CH2:30][CH2:29]1>CCOCC>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:20](=[O:21])[N:19]([CH3:22])[C:12]2[N:13]=[C:14]([NH:23][CH2:24][CH2:25][CH2:26][CH2:27][N:28]3[CH2:29][CH2:30][N:31]([CH3:34])[CH2:32][CH2:33]3)[N:15]=[CH:16][C:11]=2[CH:10]=1

参加物

4

反応物 2

HCID 64841924-(4-Methylpiperazin-1-yl)butan-1-amineHCID 107367016-(2,6-Dichlorophenyl)-8-methyl-2-(methylthio)pyrido[2,3-d]pyrimidin-7(8H)-one

生成物 1

HCID 53278792-aminopyrido[2,3-d]pyrimidin-7(8H)-one 32

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
170 °C

実験手順

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.;

後処理

  1. temperaturewas heated
  2. waitAfter 2 hours
  3. temperaturethe solution was cooled to room temperature
  4. washThe solution was washed with 4×5 mL of water
  5. washwash
  6. dry with materialThe ether solution was dried over potassium carbonate
  7. filtrationfiltered
  8. concentrationconcentrated to ca. 2 mL volume
  9. customThe crystals that separated on inducement
  10. filtrationwere filtered
  11. washwashed with ether

出典と根拠

ORDレコード
ord-93c51878ae8a413eb4db15ce380f4843
出典データセット
uspto-grants-1998_03
特許番号
US05733914

関連ノート

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