Potassium Carbonate → HCID 20506316, Verbindung

HRID 354967Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 354967
[OH:1][CH:2]1[CH2:7][CH2:6][N:5]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH2:4][CH2:3]1.[F:13][C:14]1[CH:19]=[CH:18][C:17]([CH:20]([C:22]2[CH:27]=[CH:26][C:25]([F:28])=[CH:24][CH:23]=2)Br)=[CH:16][CH:15]=1.C(=O)([O-])[O-].[K+].[K+]>O>[F:13][C:14]1[CH:15]=[CH:16][C:17]([CH:20]([C:22]2[CH:27]=[CH:26][C:25]([F:28])=[CH:24][CH:23]=2)[O:1][CH:2]2[CH2:3][CH2:4][N:5]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH2:6][CH2:7]2)=[CH:18][CH:19]=1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 676651,1'-(Bromomethylene)bis(4-fluorobenzene)HCID 96394Ethyl 4-hydroxypiperidine-1-carboxylate

Produkt 1

HCID 20506316HCID 20506316, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
140 °C

Versuchsvorschrift

A mixture of 21.5 parts of ethyl 4-hydroxy-1-piperidinecarboxylate, 35.2 parts of bis(4-fluorophenyl)bromomethane and 8.6 parts of potassium carbonate is stirred and heated in an oil-bath at 140° C. for 3 hours. The reaction mixture is allowed to cool to room temperature and water is added. The product is extracted with methylbenzene. The extract is washed successively with water, a diluted hydrochloric acid solution and a sodium bicarbonate solution, dried, filtered and evaporated. The forerun is distilled off (bp. till 143° C. at 0.5-1 mm. pressure), yielding ethyl 4-[bis(4-fluorophenyl)methoxy]-1-piperidinecarboxylate as an oily residue.

Aufarbeitung

  1. temperatureto cool to room temperature
  2. extractionThe product is extracted with methylbenzene
  3. washThe extract is washed successively with water
  4. dry with materiala diluted hydrochloric acid solution and a sodium bicarbonate solution, dried
  5. filtrationfiltered
  6. customevaporated
  7. distillationThe forerun is distilled off (bp. till 143° C. at 0.5-1 mm. pressure)

Quellen und Nachweise

ORD-Eintrag
ord-b8117dfa651246e6824c11ed9c8a7ad4
Quelldatensatz
uspto-grants-1983_03
Patentnummer
US04377578

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