1-(Thiophen-3-yl)ethanone → HCID 18936319、化合物

HRID 2819

反応式

HRID 2819 の反応式
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

参加物

6

反応物 4

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

生成物 1

HCID 18936319HCID 18936319、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒3 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7674ce8e93ec4e02859f77b6a1662375
出典データセット
uspto-grants-1998_03
特許番号
US05731335

関連ノート

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