Reaktion #2476391

Reaktionsgleichung

magnesium

hydrochloric acid

4-(1,4-dioxaspiro[4.5]dec-8-yl)cyclohexanone

ammonium chloride

p-bromopropylbenzene

→

crude product

4-(1,4-dioxaspiro[4.5]dec-8-yl)-1-(4-propylphenyl)cyclohexanol

Lösungsmittel

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONWhen the addition
2. 2
   Temperaturthe mixture is heated
3. 3
   Temperaturunder reflux for 1 h
4. 4
   workup.ADDITIONis added
5. 5
   Extraktionextracted a number of times with MTBE
6. 6
   WaschenThe combined organic phases are washed with water
7. 7
   Sonstigethe solution is dried

Vorschrift

A solution of 160 g (0.67 mol) of 4-(1,4-dioxaspiro[4.5]dec-8-yl)cyclohexanone in 600 ml of THF is added to a solution of the Grignard reagent generated from 147 g (0.74 mol) of p-bromopropylbenzene and 18.0 g (0.74 mol) of magnesium turnings (400 ml of THF). When the addition is complete, the mixture is heated under reflux for 1 h, and sat. ammonium chloride soln. is added. The mixture is acidified using dil. hydrochloric acid and extracted a number of times with MTBE. The combined organic phases are washed with water, and the solution is dried using sodium sulfate. The crude product obtained after removal of the solvents is used without further purification.

Quelle