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

HRID 12424노트

반응식

HRID 12424 반응식
[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

참가 물질

4

반응물 2

HCID 40632PirfenidoneHCID 87949Lawesson's reagent

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a5e9cfcf879a480fa44c407279407e0b
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728013B2

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