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Hydrochloric Acid → 2-ethoxy-7-methoxy-3-[4-(2,2,2-trifluoroethoxy)phenyl]pyrido[2,3-d]pyrimidin-4(3H)-one

HRID 570687
ノート
印刷プレビュー

反応式

HRID 570687 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[C:11](=[O:12])[N:10]([C:13]3[CH:18]=[CH:17][C:16]([O:19][CH2:20][C:21]([F:24])([F:23])[F:22])=[CH:15][CH:14]=3)[C:9](SCCC)=[N:8][C:7]=2[N:29]=1.[O-:30][CH2:31][CH3:32].[Na+].Cl>C(O)C>[CH2:31]([O:30][C:9]1[N:10]([C:13]2[CH:14]=[CH:15][C:16]([O:19][CH2:20][C:21]([F:22])([F:23])[F:24])=[CH:17][CH:18]=2)[C:11](=[O:12])[C:6]2[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[N:29][C:7]=2[N:8]=1)[CH3:32]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 2723922Sodium ethoxideHCID 68015336HCID 68015336、化合物

生成物 1

HCID 680153322-ethoxy-7-methoxy-3-[4-(2,2,2-trifluoroethoxy)phenyl]pyrido[2,3-d]pyrimidin-4(3H)-one収率 51.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
60 °C

実験手順

7-Methoxy-2-(propylsulfanyl)-3-[4-(2,2,2-trifluoroethoxy)phenyl]pyrido[2,3-d]pyrimidin-4(3H)-one (200 mg) was dissolved in ethanol (15 ml), sodium ethoxide (20% ethanol solution, 850 mg) was added thereto, and the mixture was stirred at 60° C. for 1 hr. The reaction mixture was poured into 0.2M hydrochloric acid (15 ml), and the precipitated precipitate was collected by filtration, and dissolved in tetrahydrofuran (15 ml). The solution was diluted with ethyl acetate (30 ml), and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the obtained residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (95 mg).

後処理

  1. filtrationthe precipitated precipitate was collected by filtration
  2. dissolutiondissolved in tetrahydrofuran (15 ml)
  3. additionThe solution was diluted with ethyl acetate (30 ml)
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. customthe obtained residue was purified by silica gel column chromatography (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-1472719d772441418b48656cd047fd1f
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09023858B2

反応ノート

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