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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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Lawesson's reagent → HCID 14424279、化合物

HRID 414224
ノート
印刷プレビュー

反応式

HRID 414224 の反応式
COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:10])=CC=1.[CH3:23][C:24]1[S:28][C:27]([C:29](=O)[CH2:30][NH:31][C:32](=O)[C:33]2[CH:38]=[CH:37][C:36]([C:39]([F:42])([F:41])[F:40])=[CH:35][CH:34]=2)=[CH:26][CH:25]=1>C1(C)C=CC=CC=1.C(Cl)Cl>[CH3:23][C:24]1[S:28][C:27]([C:29]2[S:10][C:32]([C:33]3[CH:38]=[CH:37][C:36]([C:39]([F:42])([F:41])[F:40])=[CH:35][CH:34]=3)=[N:31][CH:30]=2)=[CH:26][CH:25]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 87949Lawesson's reagentHCID 14424278HCID 14424278、化合物

生成物 1

HCID 14424279HCID 14424279、化合物収率 53.9%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒2 回HCID 6344Dichloromethane溶媒

実験手順

To a stirred suspension of Lawesson's Reagent (2.3 g, 0.0057 mole) in approximately 40 ml of toluene was added a mixture of N-[2-(5-methylthienyl)-2-oxoethyl]-4-trifluoromethylbenzamide (3.0 g, 0.011 mole) in toluene (35 ml). After complete addition the reaction mixture was heated at reflux for approximately four hours, then was allowed to cool to room temperature and stirred for two days. The solvent was removed from the reaction mixture by evaporation under reduced pressure, leaving an oil. The oil was dissolved in a small amount of methylene chloride and purified by column chromatography on silica gel, eluting with methylene chloride, yielding 1.0 g of 5-(5-methylthien-2-yl)-2-(4-trifluoromethylphenyl)thiazole as a solid, m.p. 150°-152° C.

後処理

  1. additionwas added
  2. additionAfter complete addition the reaction mixture
  3. temperaturewas heated
  4. temperatureat reflux for approximately four hours
  5. customThe solvent was removed from the reaction mixture by evaporation under reduced pressure
  6. customleaving an oil
  7. custompurified by column chromatography on silica gel
  8. washeluting with methylene chloride

出典と根拠

ORDレコード
ord-ef927fe9fdb84ec9ba860d24af4838be
出典データセット
uspto-grants-1988_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04791124

反応ノート

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