Ethyl Acetate → 2-phenylamino-8H-pyrido[2,3-d]pyrimidin-7-one

HRID 2300059ノート

反応式

HRID 2300059 の反応式
CS([C:4]1[N:5]=[CH:6][C:7]2[CH:13]=[CH:12][C:11](=[O:14])[NH:10][C:8]=2[N:9]=1)=O.CS(C1N=C[C:22]2[CH:28]=[CH:27][C:26](=O)[NH:25][C:23]=2N=1)(=O)=O.[C:30](OCC)(=O)C>NC1C=CC=CC=1>[C:23]1([NH:25][C:4]2[N:5]=[CH:6][C:7]3[CH:13]=[CH:12][C:11](=[O:14])[NH:10][C:8]=3[N:9]=2)[CH:22]=[CH:28][CH:27]=[CH:26][CH:30]=1

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 106084702-(Methylsulfinyl)pyrido[2,3-d]pyrimidin-7(1H)-oneHCID 183749342-(Methylsulfonyl)pyrido[2,3-d]pyrimidin-7(1H)-one

生成物 1

HCID 105140732-phenylamino-8H-pyrido[2,3-d]pyrimidin-7-one

試薬・触媒・溶媒 1

HCID 6115Aniline溶媒

実験手順

A suspension of 204 mg of the mixture of 2-methanesulfinyl-8H-pyrido[2,3-d]pyrimidin-7-one and 2-methanesulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one in 1 mL of aniline was heated at reflux for 10 minutes resulting in a dark brown solution. Upon cooling to room temperature, a solid formed. Ethyl acetate was added, and the solid was collected by filtration, washed with ethyl acetate, then suspended in methanol and filtered, and washed with additional methanol to provide 175 mg of 2-phenylamino-8H-pyrido[2,3-d]pyrimidin-7-one, mp>350° C.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 10 minutes
  3. customresulting in a dark brown solution
  4. customa solid formed
  5. filtrationthe solid was collected by filtration
  6. washwashed with ethyl acetate
  7. filtrationfiltered
  8. washwashed with additional methanol

出典と根拠

ORDレコード
ord-046426131380437b96579baa59856a8a
出典データセット
uspto-grants-2002_12
特許番号
US06498163B1

反応ノート

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