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1-Bromooctane → 2-Octylthio-4,5-diphenylimidazole

HRID 265376
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HRID 265376 반응식
[C:1]1([C:7]2[N:8]=[C:9]([SH:18])[NH:10][C:11]=2[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Br[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27].C(=O)([O-])[O-].[K+].[K+]>CC(=O)CC>[CH2:20]([S:18][C:9]1[NH:8][C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[C:11]([C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)[N:10]=1)[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 81401-BromooctaneHCID 11430Potassium CarbonateHCID 178527825HCID 178527825, 화합물

생성물 1

HCID 229164132-Octylthio-4,5-diphenylimidazole수율 53%

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

A mixture of 4,5-diphenyl-2-imidazolethiol (2.5 g), 8-bromooctane (3.8 g), anhydrous potassium carbonate (13.7 g) and dry butanone (60 ml) was stirred at reflux for 2 h. The cooled reaction mixture was filtered to remove solid and the filtrate was evaporated to dryness. The residue was mixed with hexane and the resulting precipitate was collected by filtration. Recrystallisation from ethanol and water gave 2-octylthio-4,5-diphenylimidazole (1.9 g, 53%) as a white solid, m.p. 133°-4°.

후처리

  1. temperatureat reflux for 2 h
  2. customThe cooled reaction mixture
  3. filtrationwas filtered
  4. customto remove solid
  5. customthe filtrate was evaporated to dryness
  6. additionThe residue was mixed with hexane
  7. filtrationthe resulting precipitate was collected by filtration
  8. customRecrystallisation from ethanol and water

출처 및 근거

ORD 기록
ord-8be18dbb57e04da4aefbd7dcf73c97b4
출처 데이터셋
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05648373

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