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Lawesson's reagent → HCID 15230377, 화합물

HRID 1708396
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HRID 1708396 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-methylphenyl)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-bd0d55127bee420d8af404b0039ee164
출처 데이터셋
uspto-grants-1994_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05358964

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