Sulfuric Acid → 4-(4-Fluorophenyl)cyclohexan-1-one

HRID 12052ノート

反応式

HRID 12052 の反応式
[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

  1. 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…