3,4-Dimethoxyaniline → 6-(2,6-Dichlorophenyl)-2-(3,4-dimethoxyphenylamino)-8-ethyl-8H-pyrido[2,3-d]pyrimidin-7-one

HRID 3206

反応式

HRID 3206 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]([CH2:24][CH3:25])[C:12]2[N:13]=[C:14](S(C)(=O)=O)[N:15]=[CH:16][C:11]=2[CH:10]=1.[CH3:26][O:27][C:28]1[CH:29]=[C:30]([CH:32]=[CH:33][C:34]=1[O:35][CH3:36])[NH2:31]>C(O)(=O)C.O>[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]([CH2:24][CH3:25])[C:12]2[N:13]=[C:14]([NH:31][C:30]3[CH:32]=[CH:33][C:34]([O:35][CH3:36])=[C:28]([O:27][CH3:26])[CH:29]=3)[N:15]=[CH:16][C:11]=2[CH:10]=1

参加物

5

反応物 2

HCID 227703,4-DimethoxyanilineHCID 105969946-(2,6-dichlorophenyl)-8-ethyl-2-methanesulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one

生成物 1

HCID 116842536-(2,6-Dichlorophenyl)-2-(3,4-dimethoxyphenylamino)-8-ethyl-8H-pyrido[2,3-d]pyrimidin-7-one

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

反応条件

温度
160 °C

実験手順

A mixture of 0.150 g (0.38 mmol) of 6-(2,6-dichlorophenyl)-8-ethyl-2-methanesulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 68 and 0.500 g (3.30 mmol) of 3,4-dimethoxyaniline was heated in a 160° C. oil bath for 5 minutes. The dark blue solution was cooled and dissolved in 2 mL of warm glacial acetic acid. This solution was diluted to 10 mL volume with water to precipitate a solid. The solid was filtered, washed well with water, and dried; wt 0.200 g. Purification was effected by filtration of an ethyl acetate (25 mL) solution through a layer of silica gel and washing the silica gel with ethyl acetate. The filtrate was concentrated to 3 mL volume. The crystals that separated on inducement were filtered and washed with 1 mL of ethyl acetate and then 1 mL of ether; wt 0.116 g; mp 221°-223° C.

後処理

  1. temperatureThe dark blue solution was cooled
  2. customto precipitate a solid
  3. filtrationThe solid was filtered
  4. washwashed well with water
  5. customdried
  6. customPurification
  7. filtrationwas effected by filtration of an ethyl acetate (25 mL) solution through a layer of silica gel
  8. washwashing the silica gel with ethyl acetate
  9. concentrationThe filtrate was concentrated to 3 mL volume
  10. customThe crystals that separated on inducement
  11. filtrationwere filtered
  12. washwashed with 1 mL of ethyl acetate

出典と根拠

ORDレコード
ord-81f4c40125694e76a49bac3d81b5f484
出典データセット
uspto-grants-1998_03
特許番号
US05733914

関連ノート

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