P-Anisidine → 6-(2,6-Dichlorophenyl)-2-(4-methoxyphenylamino)-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one

HRID 3199

반응식

HRID 3199 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:22](=[O:23])[N:21]([CH3:24])[C:12]2[N:13]=[C:14](S(C)(=O)=O)[N:15]=[CH:16][C:11]=2[CH:10]=1.[CH3:25][O:26][C:27]1[CH:33]=[CH:32][C:30]([NH2:31])=[CH:29][CH:28]=1>>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:22](=[O:23])[N:21]([CH3:24])[C:12]2[N:13]=[C:14]([NH:31][C:30]3[CH:32]=[CH:33][C:27]([O:26][CH3:25])=[CH:28][CH:29]=3)[N:15]=[CH:16][C:11]=2[CH:10]=1

참가 물질

3

반응물 2

HCID 7732P-AnisidineHCID 105961576-(2,6-Dichlorophenyl)-8-methyl-2-methylsulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one

생성물 1

HCID 53278966-(2,6-Dichlorophenyl)-2-(4-methoxyphenylamino)-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one

반응 조건

온도
180 °C

실험 절차

A mixture of 0.113 g (0.29 mmol) of 6-(2,6-dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 39 and 0.50 g (4.10 mmol) of 4-methoxyaniline was heated, with stirring, in a 180° C. oil bath. The resulting solution was heated for 10 minutes. Much of the excess aniline was evaporated at reduced pressure. The remainder was dissolved in 2 mL of ethyl acetate. The crystals that separated from the dark solution were filtered and washed with 2 mL of ethyl acetate, wt 0.102 g.

후처리

  1. temperaturewas heated
  2. temperatureThe resulting solution was heated for 10 minutes
  3. customMuch of the excess aniline was evaporated at reduced pressure
  4. dissolutionThe remainder was dissolved in 2 mL of ethyl acetate
  5. customThe crystals that separated from the dark solution
  6. filtrationwere filtered
  7. washwashed with 2 mL of ethyl acetate, wt 0.102 g

출처 및 근거

ORD 기록
ord-2385e0240fd44243a34f8caa93efa84f
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05733914

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