反应 #40330

ord-078b576691f14997974b7557469bacb0

反应方程式

Fc1ccc(C2CCC3(CC2)OCCO3)cc1
8-(4-fluor-phenyl)-1,4-dioxaspiro[4.5]decane
O=S(=O)(O)O
sulphuric acid
O=C1CCC(c2ccc(F)cc2)CC1
raw title compound
O=C1CCC(c2ccc(F)cc2)CC1
4-(4-fluorophenyl)-cyclohexanone

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取After dilution with water (12 ml) extraction

实验过程

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]+.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07727979B2uspto-grants-2010_06