Lawesson's reagent → HCID 13822014, 화합물

HRID 1731263노트

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HRID 1731263 반응식
[Cl:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([Cl:13])[CH:8]=2)[N:5]=[CH:4][C:3]=1[C:14]([NH:16][CH3:17])=O.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:27])=CC=1>C1(C)C=CC=CC=1>[Cl:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([Cl:13])[CH:8]=2)[N:5]=[CH:4][C:3]=1[C:14](=[S:27])[NH:16][CH3:17]

참가 물질

4

반응물 2

HCID 87949Lawesson's reagentHCID 1757891H-Pyrazole-4-carboxamide, 5-chloro-1-(3-chlorophenyl)-N-methyl-

생성물 1

HCID 13822014HCID 13822014, 화합물수율 56%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A solution of 3.0 g of 5-chloro-1-(3-chlorophenyl)-N-methyl-1H-pyrazole-4-carboxamide and 6.5 g of Lawesson's Reagent in 150 ml toluene was refluxed for one hour. The solution was cooled and the volatiles were removed under reduced pressure. The residue was chromatographed over silica gel eluting with methylene chloride. The fractions containing the major component were combined and the solvent was evaporated therefrom to afford 1.6 g, following recrystallization from toluene, of 5-chloro-1-(3-chlorophenyl)-N-methyl-1H-pyrazole-4-thiocarboxamide. Yield 56%. mp=128°-130° C.

후처리

  1. temperatureThe solution was cooled
  2. customthe volatiles were removed under reduced pressure
  3. customThe residue was chromatographed over silica gel eluting with methylene chloride
  4. additionThe fractions containing the major component
  5. customthe solvent was evaporated
  6. customto afford 1.6 g
  7. customrecrystallization from toluene

출처 및 근거

ORD 기록
ord-5ddbd92fd55c46fda452faf3bee0e706
출처 데이터셋
uspto-grants-1986_11
특허 번호
US04620865

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