反応式
Cl.[CH2:2]([C:4]1([CH3:14])[CH2:12][C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]1=O)[CH3:3]>O.C(O)C.[Zn].C([O-])(=O)C.[Hg+2].C([O-])(=O)C>[CH2:2]([C:4]1([CH3:14])[CH2:12][C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH2:5]1)[CH3:3]参加物
実験手順
335 g of zinc dust and 33.5 g of mercury (II) acetate and a solution of 330 cc of concentrated hydrochloric acid in 280 cc of water are rapidly added dropwise in a stirring apparatus. The mixture is boiled at reflux and a solution of 63 g of 2-ethyl-2-methyl-1-indanone in 525 cc of ethanol is added dropwise within 10 minutes while stirring. The reaction mixture is subsequently stirred at reflux for 28 hours, cooled, filtered, and the residue is washed with water/petroleum ether. The filtrate is extracted with petroleum ether, the petroleum ether extract is washed with water and dried over sodium sulphate. The crude 2-ethyl-2-methyl-indan, obtained as an oil after evaporating the solvent, is purified by chromatography on aluminium oxide/petroleum ether.
後処理
- temperatureat reflux
- stirringThe reaction mixture is subsequently stirred
- temperatureat reflux for 28 hours
- temperaturecooled
- filtrationfiltered
- washthe residue is washed with water/petroleum ether
- extractionThe filtrate is extracted with petroleum ether
- extractionthe petroleum ether extract
- washis washed with water
- dry with materialdried over sodium sulphate
出典と根拠
- ORDレコード
- ord-28adf486cf104b4d8d97dd240ed54f30
- 出典データセット
- uspto-grants-1979_08
- 特許番号
- US04166131
関連ノート
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