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

HRID 401508노트

반응식

HRID 401508 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-b4e2dcc0e8c540aa99262f8e64454dec
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08741936B2

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