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Lawesson's reagent → HCID 86002050, 화합물

HRID 1986049
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HRID 1986049 반응식
[CH3:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:11]=1[O:10][C:9]([C:12]1[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=1)=[CH:8][C:7]2=O.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:30])=CC=1>C1(C)C=CC=CC=1>[CH3:19][O:18][C:15]1[CH:16]=[CH:17][C:12]([C:9]2[O:10][C:11]3[C:6]([C:7](=[S:30])[CH:8]=2)=[CH:5][CH:4]=[CH:3][C:2]=3[CH3:1])=[CH:13][CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 87949Lawesson's reagentHCID 6886834'-Methoxy-8-methylflavone

생성물 1

HCID 86002050HCID 86002050, 화합물수율 125.9%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Compound I-23 was prepared according to the general method described above in Scheme 1. A stirred mixture of 8-methyl-4′-methoxyflavone (200.0 mg, 0.75 mmol), Lawesson's reagent (182.3 mg, 0.45 mmol) and anhydrous toluene (4.0 mL) was refluxed under N2 for 1.5 hr. The solvent was removed under vacuum and the residue was purified by silica gel chromatography (20% ethyl acetate/hexane) to give 2-(4-Methoxy-phenyl)-8-methyl-chromene-4-thione (160.0 mg, 75.5% yield) as a red solid. Thione was used in next step without further purification. LC/MS: (M+H) 283.1. LC/Method A/8.967 min, 90.0% purity by area %.

후처리

  1. customCompound I-23 was prepared
  2. temperaturewas refluxed under N2 for 1.5 hr
  3. customThe solvent was removed under vacuum
  4. customthe residue was purified by silica gel chromatography (20% ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-1c23b695185c4b8ebfc679dc150c25eb
출처 데이터셋
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07547794B2

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