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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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Sodium Hydroxide → 2-(3,5-Bis-trifluoromethyl-phenyl)-N-(6'-chloro-2-methyl-[3,4]bipyridinyl-3'-yl)-N-methyl-isobutyramide

HRID 347691
ノート
印刷プレビュー

反応式

HRID 347691 の反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([NH:8][CH3:9])=[C:4]([C:10]2[C:11]([CH3:16])=[N:12][CH:13]=[CH:14][CH:15]=2)[CH:3]=1.C([Li])CCC.[F:22][C:23]([F:41])([F:40])[C:24]1[CH:25]=[C:26]([C:34]([CH3:39])([CH3:38])[C:35](Cl)=[O:36])[CH:27]=[C:28]([C:30]([F:33])([F:32])[F:31])[CH:29]=1.[OH-].[Na+]>C1COCC1>[F:33][C:30]([F:31])([F:32])[C:28]1[CH:27]=[C:26]([C:34]([CH3:38])([CH3:39])[C:35]([N:8]([C:5]2[CH:6]=[N:7][C:2]([Cl:1])=[CH:3][C:4]=2[C:10]2[C:11]([CH3:16])=[N:12][CH:13]=[CH:14][CH:15]=2)[CH3:9])=[O:36])[CH:25]=[C:24]([C:23]([F:40])([F:22])[F:41])[CH:29]=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 14798Sodium HydroxideHCID 112671412-(3,5-Bis(trifluoromethyl)phenyl)-2-methylpropanoyl chlorideHCID 586946066'-Chloro-N,2-dimethyl-[3,4'-bipyridin]-3'-amineHCID 178418339Butyllithium

生成物 1

HCID 210836352-(3,5-Bis-trifluoromethyl-phenyl)-N-(6'-chloro-2-methyl-[3,4]bipyridinyl-3'-yl)-N-methyl-isobutyramide収率 73%

試薬・触媒・溶媒

1
HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 0.19 g (0.81 mmol) (6′-chloro-2-methyl-[3,4′]bipyridinyl-3′-yl)-methyl-amine in 8 ml THF were added 0.52 ml (0.83 mmol) of a 1.6 M solution of n-butyllithium in hexanes at −78° C. After 15 min 0.28 g (0.88 mmol) 2-(3,5-bis-trifluoromethyl-phenyl)-2-methyl-propionyl chloride were added. The reaction mixture was allowed to warm to room temperature during 30 min. After addition of a 0.2 M aqueous sodium hydroxide solution the mixture was extracted with three portions of dichloromethane. The combined organic layers were dried over sodium sulfate and concentrated. Flash chromatography gave 0.30 g (73%) of the title compound.

後処理

  1. extractionwas extracted with three portions of dichloromethane
  2. dry with materialThe combined organic layers were dried over sodium sulfate
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-10ef493617644c5e9c05a8790083ef81
出典データセット
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07176205B2

反応ノート

読み込み中…

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