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

HRID 401508ノート

反応式

HRID 401508 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-b4e2dcc0e8c540aa99262f8e64454dec
出典データセット
uspto-grants-2014_06
特許番号
US08741936B2

反応ノート

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