2-Methoxyaniline → 6-(2,6-dichlorophenyl)-2-[(2-methoxyphenyl)amino]-8-methyl-7H,8H-pyrido[2,3-d]pyrimidin-7-one

HRID 3202

반응식

HRID 3202 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][CH:31]=[CH:30][C:28]=1[NH2:29]>CCOCC>[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:29][C:28]3[CH:30]=[CH:31][CH:32]=[CH:33][C:27]=3[O:26][CH3:25])[N:15]=[CH:16][C:11]=2[CH:10]=1

참가 물질

4

반응물 2

HCID 70002-MethoxyanilineHCID 105961576-(2,6-Dichlorophenyl)-8-methyl-2-methylsulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one

생성물 1

HCID 53278946-(2,6-dichlorophenyl)-2-[(2-methoxyphenyl)amino]-8-methyl-7H,8H-pyrido[2,3-d]pyrimidin-7-one

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
175 °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 2-methoxyaniline was heated, with stirring, in a 175° C. oil bath. The resulting solution was heated for 5 minutes and cooled to room temperature. Ether (2 mL) was added. The crystals that developed were filtered and washed with 1 mL of ether; wt 0.070 g. The solid was purified to remove dark colors by silica gel chromatography, eluting with chloroform. Recrystallization from ether gave pure product; wt 0.029 g; mp 200°-201° C.

후처리

  1. temperaturewas heated
  2. temperatureThe resulting solution was heated for 5 minutes
  3. temperaturecooled to room temperature
  4. filtrationThe crystals that developed were filtered
  5. washwashed with 1 mL of ether
  6. customThe solid was purified
  7. customto remove dark colors by silica gel chromatography
  8. washeluting with chloroform
  9. customRecrystallization from ether
  10. customgave pure product

출처 및 근거

ORD 기록
ord-2a5b023190f34924a6abcd11c41e178a
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05733914

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