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

HRID 3199

反応式

HRID 3199 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: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

参加物

3

反応物 2

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

生成物 1

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

反応条件

温度
180 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2385e0240fd44243a34f8caa93efa84f
出典データセット
uspto-grants-1998_03
特許番号
US05733914

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