Reaktion #353835

Reaktionsgleichung

water

sodium hydride

trans-4-(trans-4-propylcyclohexyl)cyclohexanol

4-methoxybenzyl chloride

→

trans-4-(trans-4-propylcyclohexyl)cyclohexyl-4-methoxybenzyl ether

Lösungsmittel

N,N-dimethylformamide

N,N-dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGto stirring at 50° C. for one hour
2. 2
   workup.STIRRINGthe mixture was stirred
3. 3
   Sonstigereacted at the same temperature for 3 hours
4. 4
   workup.STIRRINGwith stirring
5. 5
   workup.ADDITIONwas added to the reaction mixture
6. 6
   Extraktionthe mixture was extracted with toluene
7. 7
   Waschenwashed with a saturated NaCl aqua
8. 8
   Sonstigedried
9. 9
   Sonstigethe solvent was removed under reduced pressure
10. 10
    SonstigeThe residue was purified by silica gel column

Vorschrift

To 0.6 g of sodium hydride (purity 60%) was added 30 ml of anhydrous N,N-dimethylformamide. While stirring sufficiently, to the solution was added a solution of 3.36 g of trans-4-(trans-4-propylcyclohexyl)cyclohexanol dissolved in 10 ml of anhydrous N,N-dimethylformamide. This mixture was continued to stirring at 50° C. for one hour and then 2.8 g of 4-methoxybenzyl chloride was added thereto, and the mixture was stirred and reacted at the same temperature for 3 hours with stirring. After completion of the reaction, 100 ml of water was added to the reaction mixture, the mixture was extracted with toluene, washed with a saturated NaCl aqua, dried and the solvent was removed under reduced pressure. The residue was purified by silica gel column to obtain 1.0 g of the targeted trans-4-(trans-4-propylcyclohexyl)cyclohexyl-4-methoxybenzyl ether.

Quelle