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2-Thiophenecarbonyl chloride → HCID 15917157、化合物

HRID 2229822
ノート
印刷プレビュー

反応式

HRID 2229822 の反応式
[S-:1][C:2]#[N:3].[K+].[S:5]1[CH:9]=[CH:8][CH:7]=[C:6]1[C:10](Cl)=[O:11]>CC(C)=O>[S:5]1[CH:9]=[CH:8][CH:7]=[C:6]1[C:10]([N:3]=[C:2]=[S:1])=[O:11]
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 789282-Thiophenecarbonyl chlorideHCID 516872Potassium thiocyanate

生成物 1

HCID 15917157HCID 15917157、化合物収率 53%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a freshly prepared solution of potassium thiocyanate (2.14 g, 22 mmol) in dry acetone (80 ml ), thiophene-2-carbonyl chloride (2.93 g, 20 mmol) was added dropwise at room temperature; the reaction mixture was then heated under a reflux for 15 min to give thiophene-2-carbonyl isothiocyanate in situ as a yellow suspension. The heating was stopped and 2-imidazolidinethione (2.04 g, 20 mmol) was added. The mixture was then heated under reflux for an additional 4 hours before being allowed to cool followed by stirring at room temperature overnight (15 hours). 50 ml of water was added and the mixture was further stirred at room temperature for a few minutes. The resulting precipitate was collected by filtration and washed with water, water/methanol (1:1) and methanol to give the compound ARE111 (2.865 g, yield=53%)

後処理

  1. temperaturethe reaction mixture was then heated under
  2. temperaturea reflux for 15 min

出典と根拠

ORDレコード
ord-70422e9dbbe64ea3ba33ee489bf5f9ae
出典データセット
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06420563B1

反応ノート

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