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3-Pyridinemethanol → HCID 53682346、化合物

HRID 1200056
ノート
印刷プレビュー

反応式

HRID 1200056 の反応式
[S:1]1[CH:5]=[C:4]([CH:6]=[CH:7][C:8]2[S:12][C:11]([C:13](Cl)=[O:14])=[CH:10][CH:9]=2)[C:3]2[CH:16]=[CH:17][CH:18]=[CH:19][C:2]1=2.N1C=CC=C(C[OH:27])C=1>N1C=CC=CC=1>[S:1]1[CH:5]=[C:4]([CH:6]=[CH:7][C:8]2[S:12][C:11]([C:13]([OH:27])=[O:14])=[CH:10][CH:9]=2)[C:3]2[CH:16]=[CH:17][CH:18]=[CH:19][C:2]1=2
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 75103-PyridinemethanolHCID 539913705-[2-(Benzo[b]thiophen-3-yl)ethenyl]thiophene-2-carboxylic acid chloride

生成物 1

HCID 53682346HCID 53682346、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

The acid chloride of 5-[2-(benzo[b]thiophen-3-yl)ethenyl]thiophene-2-carboxylic acid was prepared as described in Example 9. To a suspension of 5-[2-(benzo[b]thiophen-3-yl)ethenyl]thiophene2-carboxylic acid chloride (5.00 g) and pyridine (50 ml) was added 3-pyridylcarbinol (1.79 g). After refluxing overnight, the mixture was evaporated, and the residue was dissolved in ether, filtered, and concentrated. The residue was purified by high performance liquid chromatography (silica gel, eluted with 2:1 ethyl acetate:hexane). The appropriate fractions were combined and evaporated. The residue was recrystallized from toluene/hexane to afford 1.4 g (23%) of the product, mp 97°-98° C.

後処理

  1. temperatureAfter refluxing overnight
  2. customthe mixture was evaporated
  3. dissolutionthe residue was dissolved in ether
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue was purified by high performance liquid chromatography (silica gel, eluted with 2:1 ethyl acetate:hexane)
  7. customevaporated
  8. customThe residue was recrystallized from toluene/hexane

出典と根拠

ORDレコード
ord-1592a9c9c70a4632af2721e3e6f41298
出典データセット
uspto-grants-1990_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04904674

反応ノート

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