Pirfenidone → 2(1H)-Pyridinethione, 5-methyl-1-phenyl-

HRID 12424ノート

反応式

HRID 12424 の反応式
[C:1]1([N:7]2[CH:12]=[C:11]([CH3:13])[CH:10]=[CH:9][C:8]2=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:24])=CC=1>C1(C)C=CC=CC=1>[C:1]1([N:7]2[CH:12]=[C:11]([CH3:13])[CH:10]=[CH:9][C:8]2=[S:24])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

4

反応物 2

HCID 40632PirfenidoneHCID 87949Lawesson's reagent

生成物 1

HCID 119889472(1H)-Pyridinethione, 5-methyl-1-phenyl-

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

1-phenyl-5-methyl-2-pyridinone (555.7 mg, 3 mmol) was reacted with Lawesson's reagent (606.7 mg, 1.5 mmol) in toluene (5 ml) at 90° C. Reaction mixture was evaporated and the target compound was isolated by column chromatography (20-30% ethyl acetate-hexane) followed by crystallization from methyl-tert-butyl ether. Yield 403 mg (67%), yellow solid. The 1H NMR spectra was consistent with the structure of Compound 18.

後処理

  1. customReaction mixture
  2. customwas evaporated
  3. customthe target compound was isolated by column chromatography (20-30% ethyl acetate-hexane)
  4. customfollowed by crystallization from methyl-tert-butyl ether

出典と根拠

ORDレコード
ord-a5e9cfcf879a480fa44c407279407e0b
出典データセット
uspto-grants-2010_06
特許番号
US07728013B2

反応ノート

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