N-(3-Aminopropyl)morpholine → 6-(2,6-dichlorophenyl)-8-methyl-2-{[3-(morpholin-4-yl)propyl]amino}-7H,8H-pyrido[2,3-d]pyrimidin-7-one

HRID 3188

反応式

HRID 3188 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][N:27]1[CH2:32][CH2:31][O:30][CH2:29][CH2:28]1>CN(C)C=O>[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][N:27]3[CH2:32][CH2:31][O:30][CH2:29][CH2:28]3)[N:15]=[CH:16][C:11]=2[CH:10]=1

参加物

4

反応物 2

HCID 61055N-(3-Aminopropyl)morpholineHCID 107367016-(2,6-Dichlorophenyl)-8-methyl-2-(methylthio)pyrido[2,3-d]pyrimidin-7(8H)-one

生成物 1

HCID 53278776-(2,6-dichlorophenyl)-8-methyl-2-{[3-(morpholin-4-yl)propyl]amino}-7H,8H-pyrido[2,3-d]pyrimidin-7-one

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
125 °C

実験手順

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, 1.00 g (6.90 mmol) of N-(3-aminopropyl)morpholine and 0.5 mL of dimethylformamide was heated with stirring in a 125° C. oil bath. After 2 minutes, solution was complete. After 1.5 hours, the excess amine and dimethylformamide were evaporated at reduced pressure and the residue was triturated with 5 mL of water. The gum was dissolved in 25 mL of ethyl acetate, and the solution was washed with 2×5 mL of water, dried (potassium carbonate), and concentrated. Upon dissolution in 5 mL of ether, crystals of pure product separated; wt 0.101 g; mp 140°-142° C.

後処理

  1. temperaturewas heated
  2. waitAfter 1.5 hours
  3. customthe excess amine and dimethylformamide were evaporated at reduced pressure
  4. customthe residue was triturated with 5 mL of water
  5. dissolutionThe gum was dissolved in 25 mL of ethyl acetate
  6. washthe solution was washed with 2×5 mL of water
  7. dry with materialdried (potassium carbonate)
  8. concentrationconcentrated
  9. dissolutionUpon dissolution in 5 mL of ether
  10. customcrystals of pure product separated

出典と根拠

ORDレコード
ord-ed41f375aaff41018a80d7b0ecb415a0
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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