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Lawesson's reagent → HCID 14424279, 화합물

HRID 414224
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HRID 414224 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 87949Lawesson's reagentHCID 14424278HCID 14424278, 화합물

생성물 1

HCID 14424279HCID 14424279, 화합물수율 53.9%

시약·촉매·용매 2

HCID 1140Toluene용매2회HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ef927fe9fdb84ec9ba860d24af4838be
출처 데이터셋
uspto-grants-1988_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04791124

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