1-(Thiophen-3-yl)ethanone → HCID 18936319, 화합물

HRID 2819

반응식

HRID 2819 반응식
C([Li])CCC.C[Si](C)(C)[C:8]1[S:9][CH:10]=[CH:11][N:12]=1.[C:15]([C:18]1[CH:22]=[CH:21][S:20][CH:19]=1)(=[O:17])[CH3:16].C(=O)([O-])O.[Na+]>C(OCC)C>[S:9]1[C:10]([C:15]([C:18]2[CH:22]=[CH:21][S:20][CH:19]=2)([OH:17])[CH3:16])=[CH:11][N:12]=[CH:8]1

참가 물질

6

반응물 4

HCID 151161-(Thiophen-3-yl)ethanoneHCID 516892Sodium BicarbonateHCID 5884532-TrimethylsilylthiazoleHCID 178418339Butyllithium

생성물 1

HCID 18936319HCID 18936319, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매3회

실험 절차

n-Butyllithium (2.5M solution in hexane, 5.6 ml) in diethylether (25 ml) was stirred at -70° C. under a nitrogen atmosphere and 2-trimethylsilylthiazole (2 g) in diethylether (25 ml) was added dropwise. After 30 minutes 3-acetylthiophene (1.93 g) in diethylether (25 ml) was added dropwise. After a further 45 minutes the mixture was allowed to warm to room temperature and then left to stir for a further 1 hour. Saturated aqueous sodium hydrogen carbonate was added and the organic layer was separated. The aqueous layer was extracted with diethylether. The organic layers were combined, washed, dried and evaporated and the residue was purified by flash chromatography to give the title compound as an oil.

후처리

  1. waitleft
  2. customthe organic layer was separated
  3. extractionThe aqueous layer was extracted with diethylether
  4. washwashed
  5. customdried
  6. customevaporated
  7. customthe residue was purified by flash chromatography

출처 및 근거

ORD 기록
ord-7674ce8e93ec4e02859f77b6a1662375
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05731335

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