Potassium Hydroxide → HCID 13145802, Verbindung

HRID 1074545Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1074545
[OH-].[K+].[F:3][C:4]1[CH:5]=[C:6]([CH:16]=[CH:17][CH:18]=1)[CH2:7][O:8][C:9]1[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=1.Cl[CH2:20][CH2:21][CH2:22][N:23]1[CH2:28][CH2:27][O:26][CH2:25][CH2:24]1>C(O)C>[F:3][C:4]1[CH:5]=[C:6]([CH:16]=[CH:17][CH:18]=1)[CH2:7][O:8][C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:20][CH2:21][CH2:22][N:23]2[CH2:28][CH2:27][O:26][CH2:25][CH2:24]2)=[CH:11][CH:10]=1

Komponenten

5

Edukt 3

HCID 14797Potassium HydroxideHCID 958344-(3-Chloropropyl)morpholineHCID 13145801HCID 13145801, Verbindung

Produkt 1

HCID 13145802HCID 13145802, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

To a solution of 0.56 g (0.01 mol) of potassium hydroxide in 18 ml of absolute ethanol are added 2.18 g (0.01 mol) of 4-(3-fluorobenzyloxy)phenol. There is then added a solution of 1.64 g (0.01 mol) of N-(3-chloropropyl)morpholine in 2 ml of absolute ethanol. The mixture is stirred at reflux for 24 hours, allowed to cool and then refrigerated. The solid which forms is collected by filtration, washed with absolute ethanol and dissolved in diethyl ether. The ethereal solution is washed consecutively with water (20 ml), 10% aqueous sodium hydroxide (3×15 ml) and water until neutral to litmus. The solution is dried over sodium sulfate, filtered and evaporated and recrystallized from diethyl ether-petroleum ether and from diethyl ether alone to yield N-[3-(4-{3-fluorobenzyloxy}phenoxy)propyl]morpholine.

Aufarbeitung

  1. temperatureat reflux for 24 hours
  2. temperatureto cool
  3. filtrationThe solid which forms is collected by filtration
  4. washwashed with absolute ethanol
  5. dissolutiondissolved in diethyl ether
  6. washThe ethereal solution is washed consecutively with water (20 ml), 10% aqueous sodium hydroxide (3×15 ml) and water until neutral to litmus
  7. dry with materialThe solution is dried over sodium sulfate
  8. filtrationfiltered
  9. customevaporated
  10. customrecrystallized from diethyl ether-petroleum ether and from diethyl ether alone

Quellen und Nachweise

ORD-Eintrag
ord-c72717f097ab4d5d86c01c5367f111de
Quelldatensatz
uspto-grants-1983_07
Patentnummer
US04393061

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