Lawesson's reagent → HCID 13822014、化合物

HRID 1731263ノート

反応式

HRID 1731263 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 13822014HCID 13822014、化合物収率 56%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5ddbd92fd55c46fda452faf3bee0e706
出典データセット
uspto-grants-1986_11
特許番号
US04620865

反応ノート

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