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

HRID 2300059노트

반응식

HRID 2300059 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6115Aniline용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-046426131380437b96579baa59856a8a
출처 데이터셋
uspto-grants-2002_12
특허 번호
US06498163B1

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