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Sodium methanethiolate → 6-Methylsulfanyl-[2,2']bipyridin-3-ol

HRID 228803
ノート
印刷プレビュー

反応式

HRID 228803 の反応式
F[C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][N:9]=2)[C:5]([O:14]C)=[CH:4][CH:3]=1.[CH3:16][S-:17].[Na+]>CN(C)C=O>[CH3:16][S:17][C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][N:9]=2)[C:5]([OH:14])=[CH:4][CH:3]=1
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

4

反応物 2

HCID 4378561Sodium methanethiolateHCID 688295916-Fluoro-3-methoxy-[2,2']bipyridine

生成物 1

HCID 1363851056-Methylsulfanyl-[2,2']bipyridin-3-ol収率 47%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
160 °C

実験手順

6-Fluoro-3-methoxy-[2,2′]bipyridine (12 mg) and sodium thiomethoxide (41 mg) were suspended in N,N-dimethylformamide (1.5 ml), and the suspension was stirred at 160° C. overnight. The reaction solution was cooled to room temperature, the reaction solution was then filtered, and the solvent was removed from the filtrate by distillation under the reduced pressure. The residue was purified by thin layer chromatography using acetone-chloroform to give 6-methylsulfanyl-[2,2′]bipyridin-3-ol (6 mg, yield 47%).

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート

後処理

  1. temperatureThe reaction solution was cooled to room temperature
  2. filtrationthe reaction solution was then filtered
  3. customthe solvent was removed from the filtrate by distillation under the reduced pressure
  4. customThe residue was purified by thin layer chromatography

出典と根拠

ORDレコード
ord-fca730f4c80049ef8a80896a37a8cb98
出典データセット
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07560558B2

反応ノート

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