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Ethanol → HCID 178513359, 화합물

HRID 2197438
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HRID 2197438 반응식
[O-]CC.[Na+].Cl.[NH2:6][OH:7].C(O)C.[S:11]1[CH:15]=[CH:14][CH:13]=[C:12]1[C:16]#[N:17]>C1CCCCC1.CCCCC>[OH:7][NH:6][C:16]([C:12]1[S:11][CH:15]=[CH:14][CH:13]=1)=[NH:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 702EthanolHCID 660872-ThiophenecarbonitrileHCID 443297Hydroxyamine hydrochlorideHCID 2723922Sodium ethoxide

생성물 1

HCID 178513359HCID 178513359, 화합물

시약·촉매·용매 1

HCID 21949758Cyclohexane pentane용매

실험 절차

A solution of sodium ethoxide (21% by weight in ethanol, 64.9 ml, 0.174 mol, 1.1 eq.), hydroxylamine hydrochloride (12.1 g, 0.174 mol, 1.1 eq.) and ethanol (100 ml) was refluxed for 30 minutes. Thiophene-2-carbonitrile (18.8 g; 0.172 mol; 1 eq.) was then added and the solution was refluxed continuously for 18 hours. The reaction was monitored by thin layer chromatography (TLC) (50/50 cyclohexane/pentane). The solution was evaporated under reduced pressure and the residue obtained triturated in water at pH 7. The aqueous phase, saturated beforehand with NaCl, was then extracted with ethyl ether (three times). The organic phases were combined, dried over MgSO4 and concentrated under reduced pressure to give a white powder.

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후처리

  1. temperaturethe solution was refluxed continuously for 18 hours
  2. customThe solution was evaporated under reduced pressure
  3. customthe residue obtained
  4. customtriturated in water at pH 7
  5. extractionwas then extracted with ethyl ether (three times)
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated under reduced pressure
  8. customto give a white powder

출처 및 근거

ORD 기록
ord-11c1277f76704e73836f23feea079440
출처 데이터셋
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08338599B2

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