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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Water → HCID 86685360、化合物

HRID 570697
ノート
印刷プレビュー

反応式

HRID 570697 の反応式
[H-].[Na+].[F:3][C:4]([F:10])([CH2:7][O:8][CH3:9])[CH2:5][OH:6].C(S[C:15]1[N:16]([C:27]2[CH:32]=[CH:31][C:30]([O:33][CH2:34][C:35]([F:38])([F:37])[F:36])=[CH:29][CH:28]=2)[C:17](=[O:26])[C:18]2[CH:24]=[CH:23][C:22](=[O:25])[NH:21][C:19]=2[N:20]=1)CC.O>O1CCCC1>[F:3][C:4]([F:10])([CH2:7][O:8][CH3:9])[CH2:5][O:6][C:15]1[N:16]([C:27]2[CH:32]=[CH:31][C:30]([O:33][CH2:34][C:35]([F:36])([F:38])[F:37])=[CH:29][CH:28]=2)[C:17](=[O:26])[C:18]2[CH:24]=[CH:23][C:22](=[O:25])[NH:21][C:19]=2[N:20]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 866619421247089-57-1HCID 866853582-(propylsulfanyl)-3-[4-(2,2,2-trifluoroethoxy)phenyl]pyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione

生成物 1

HCID 86685360HCID 86685360、化合物収率 4.3%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

To a suspension of sodium hydride (60% in oil, 29 mg) in tetrahydrofuran (5 ml) was added 2,2-difluoro-3-methoxypropan-1-ol (151 mg) at room temperature, and the mixture was stirred at room temperature for 10 min. To the reaction mixture was added 2-(propylsulfanyl)-3-[4-(2,2,2-trifluoroethoxy)phenyl]pyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione (165 mg), and the mixture was stirred at room temperature for 5 hr. The reaction mixture was added to water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane), and recrystallized from a mixed solvent of hexane/ethyl acetate to give the title compound (8 mg).

後処理

  1. stirringthe mixture was stirred at room temperature for 5 hr
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe extract was washed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)
  7. customrecrystallized from a mixed solvent of hexane/ethyl acetate

出典と根拠

ORDレコード
ord-559d34b6ea3a44a2a78a3ccf7e613ee5
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

読み込み中…

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