Sulfuric Acid → 4-(4-Fluorophenyl)cyclohexan-1-one
反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[CH2:17][CH2:16][C:11]3(OCC[O:12]3)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1.S(=O)(=O)(O)O>O1CCOCC1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]2[CH2:9][CH2:10][C:11](=[O:12])[CH2:16][CH2:17]2)=[CH:6][CH:7]=1参加物
4
実験手順
8-(4-fluor-phenyl)-1,4-dioxaspiro[4.5]decane (2 mmol) is dissolved in dioxane (6.5 ml) and treated with 3 ml 50% aqueous sulphuric acid accompanied by stirring at room temperature for 5 hours. After dilution with water (12 ml) extraction is carried out twice with dichloromethane. The raw title compound is obtained from the combined organic phases after drying over sodium sulphate and evaporating-off of the solvent in a vacuum (Tetrahedron 1998, 54, 15509-15524): tR 3.44 min (LC-1); ESI-MS(+): m/z 193.29 [M+H]+.
後処理
- extractionAfter dilution with water (12 ml) extraction
出典と根拠
- ORDレコード
- ord-078b576691f14997974b7557469bacb0
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07727979B2
反応ノート
読み込み中…