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Potassium Fluoride → HCID 15811458、化合物

HRID 556141
ノート
印刷プレビュー

反応式

HRID 556141 の反応式
C[Si]([C:5]#[C:6][C:7]1[CH:8]=[CH:9][C:10]([C:13]2[CH:18]=[CH:17][C:16]([C:19]#[C:20][Si](C)(C)C)=[CH:15][N:14]=2)=[N:11][CH:12]=1)(C)C.[F-].[K+]>CO>[C:19]([C:16]1[CH:17]=[CH:18][C:13]([C:10]2[CH:9]=[CH:8][C:7]([C:6]#[CH:5])=[CH:12][N:11]=2)=[N:14][CH:15]=1)#[CH:20]
参加物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 522689Potassium FluorideHCID 52476625,5'-Bis(trimethylsilylethynyl)-2,2'-bipyridine

生成物 1

HCID 15811458HCID 15811458、化合物収率 85.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Subsequently, the obtained 5,5′-bis(trimethylsilylethynyl)-2,2′-bipyridyl (120 mg, 0.34 mmol) and potassium fluoride (KF: 42 mg, 0.72 mmol) were added with dist. methanol (MeOH: 12 mL). The resultant mixture was then stirred under a nitrogen atmosphere at room temperature for 11 hours to obtain a reaction mixture. After that, an organic layer in the reaction mixture was then concentrated to obtain a crude product (II). Subsequently, the obtained crude product (II) was separated and purified by silica gel column chromatography (CH2Cl2=100) to obtain 5,5′-diethynyl-2,2′-bipyridyl (59.5 mg, 85% yield (in two steps)).

後処理

  1. customto obtain a reaction mixture
  2. concentrationAfter that, an organic layer in the reaction mixture was then concentrated
  3. customto obtain a crude product (II)
  4. customSubsequently, the obtained crude product (II)
  5. customwas separated
  6. custompurified by silica gel column chromatography (CH2Cl2=100)

出典と根拠

ORDレコード
ord-d8eb6f44f47f480fb4c8db71a8ae96af
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08053588B2

反応ノート

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