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Lawesson's reagent → HCID 15230377, 화합물

HRID 1941323
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HRID 1941323 반응식
[Cl:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[C:4]([Cl:9])[C:3]=1[NH:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1/[CH:17]=[C:18]1/[C:19](=O)[O:20][CH2:21][CH2:22]/1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:33])=CC=1>C1(C)C=CC=CC=1>[Cl:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[C:4]([Cl:9])[C:3]=1[NH:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1/[CH:17]=[C:18]1/[C:19](=[S:33])[O:20][CH2:21][CH2:22]/1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 87949Lawesson's reagentHCID 9950191HCID 9950191, 화합물

생성물 1

HCID 15230377HCID 15230377, 화합물수율 75.9%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A solution of (E)-3-[[2-[(2,6-dichloro-3-methyl-phenyl) amino]phenyl]methylene]-4,5-dihydro-2(3H)-furanone (386 mg, 1.11 mmol) and Lawesson's Reagent (273 mg, 0.68 mmol) in 15 mL of toluene is heated at reflux for 1.5 hours. The solution is concentrated in vacuo and purified by flash chromatography eluting with hexane:ethyl acetate (3:1) to provide 188 mg (47%) of (E)-3-[[2-[(2,6-dichloro-3-methylphenyl)amino]-phenyl]methylene]-4,5-dihydro-2(3H)-furanthione; mp=163°-165° C. dec.

후처리

  1. temperatureat reflux for 1.5 hours
  2. concentrationThe solution is concentrated in vacuo
  3. custompurified by flash chromatography
  4. washeluting with hexane:ethyl acetate (3:1)

출처 및 근거

ORD 기록
ord-efc5f0135f0a4b7bbd6c436e72684795
출처 데이터셋
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05703119

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