Reaktionsgleichung
[H-].[Na+].[CH2:3]([C@H:6]1[CH2:11][CH2:10][C@H:9](O)[CH2:8][CH2:7]1)[CH2:4][CH3:5].[F:13][C:14]1[CH:15]=[C:16]([CH:19]=[CH:20][C:21]=1[F:22])[CH2:17]Br.O.CN([CH:27]=[O:28])C>>[CH2:3]([C@H:6]1[CH2:11][CH2:10][C@H:9]([CH:17]([O:28][CH:27]([C@H:9]2[CH2:10][CH2:11][C@H:6]([CH2:3][CH2:4][CH3:5])[CH2:7][CH2:8]2)[C:19]2[CH:16]=[CH:15][C:14]([F:13])=[C:21]([F:22])[CH:20]=2)[C:16]2[CH:19]=[CH:20][C:21]([F:22])=[C:14]([F:13])[CH:15]=2)[CH2:8][CH2:7]1)[CH2:4][CH3:5]Komponenten
Versuchsvorschrift
0.6 g of sodium hydride (60%) was added to 30 ml of anhydrous N,N'-dimethylformamide. While stirring sufficiently, to the solution was added a solution of 2.13 g of trans-4-propylcyclohexanol dissolved in 10 ml of anhydrous N,N'-dimethylformamide. This mixture was continued to stirring at 50° C. for one hour and then 3.1 g of 3,4-difluorobenzyl bromide was added thereto, and the reaction was carried out 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 trans-4-propylcyclohexyl-3,4-difluorobenzyl ether.
Aufarbeitung
- stirringto stirring at 50° C. for one hour
- stirringwith stirring
- additionwas added to the reaction mixture
- extractionthe mixture was extracted with toluene
- washwashed with a saturated NaCl aqua
- customdried
- customthe solvent was removed under reduced pressure
- customThe residue was purified by silica gel column
Quellen und Nachweise
- ORD-Eintrag
- ord-bb5401eca14f4502884c67e7c5ec9eaf
- Quelldatensatz
- uspto-grants-1997_07
- Patentnummer
- US05651919
Verknüpfte Notizen
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