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Potassium Carbonate → HCID 178420396, Verbindung

HRID 634770
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 634770
[H-].[H-].[H-].[H-].[Li+].[Al+3].[OH-].[Na+].[CH2:9]([O:16][C:17]1[CH:22]=[CH:21][C:20]([C@H:23]2[CH2:28][CH2:27][C@H:26]([NH2:29])[CH2:25][CH2:24]2)=[CH:19][CH:18]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.[O:30]([CH2:37][CH2:38]Br)[C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1.C([O-])([O-])=O.[K+].[K+]>C1COCC1.CC(=O)CC.O>[CH2:9]([O:16][C:17]1[CH:18]=[CH:19][C:20]([C@@H:23]2[CH2:28][CH2:27][C@H:26]([NH:29][CH2:38][CH2:37][O:30][C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=3)[CH2:25][CH2:24]2)=[CH:21][CH:22]=1)[C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1.[CH2:9]([O:16][C:17]1[CH:18]=[CH:19][C:20]([C@H:23]2[CH2:28][CH2:27][C@H:26]([NH:29][CH2:38][CH2:37][O:30][C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=3)[CH2:25][CH2:24]2)=[CH:21][CH:22]=1)[C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

10

Edukt 5

HCID 11430Potassium CarbonateHCID 14798Sodium HydroxideHCID 68526Benzene, (2-bromoethoxy)-HCID 21226445Aluminium lithium hydrideHCID 178511501HCID 178511501, Verbindung

Produkt 2

HCID 178420396HCID 178420396, Verbindung
HCID 178420397
HCID 178420397, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittel2×HCID 6569Methyl Ethyl KetoneLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A mixture of 4-(4-benzyloxy-phenyl)-cyclohexanone (8.2 g, 29 mmol), benzyloxyhydroxylamine hydrochloride (4.7 g, 29 mmol) and ethanol was heated for 2 h. at reflux. The solvent was removed and the residue was crystallized to give white crystals (10.2 g, 90%) of the benzyloxy-oxime of 4-(4-benzyloxy-phenyl)-cyclohexanone. The latter was refluxed for 4 days with LiAlH4 (4 g, 105 mmol) in THF (300 ml). After the addition of H2O (30 ml), NaOH 15% (30 ml) and H2O (30 ml), the solids were removed by filtration and the filtrate evaporated. The residue was partioned between H2O and methylene chloride and the organic layer was dried and evaporated. The residue was purified by chromatography (SiO2, CH2Cl2—MeOH—aq.NH3 140:10:1) to give a mixture of cis and trans 4-(4-benzyloxy-phenyl)-cyclohexyl-amine (3.8 g) which was not separated at this stage. A portion of this mixture (1 g, 3.5 mmol) together with 2-phenoxyethyl bromide (0.78 g, 3.55 mmol), K2CO3 (1 g) and 2-butanone (20 ml) was refluxed for 3 days. The mixture was evaporated and H2O was added. Extraction with CH2Cl2 gave after drying and evaporation of the solvent a residue which was purified by chromatography (SiO2, CH2Cl2—MeOH 98:2) to give cis-[4-(4-benzyloxy-phenyl)-cyclohexyl]-(2-phenoxy-ethyl)-amine (140 mg, colorless oil, MS: m/e=402.5 (M+H+)) and trans-[4-(4-benzyloxy-phenyl)-cyclohexyl]-(2-phenoxy-ethyl)-amine (200 mg, white solid, Mp. 95-98°, MS: m/e=402.5 (M+H+)).

Aufarbeitung

  1. customthe solids were removed by filtration
  2. customthe filtrate evaporated
  3. customthe organic layer was dried
  4. customevaporated
  5. customThe residue was purified by chromatography (SiO2, CH2Cl2—MeOH—aq.NH3 140:10:1)
  6. customto give
  7. customwas not separated at this stage
  8. customThe mixture was evaporated
  9. additionH2O was added
  10. extractionExtraction with CH2Cl2
  11. customgave
  12. customafter drying
  13. customevaporation of the solvent a residue which
  14. customwas purified by chromatography (SiO2, CH2Cl2—MeOH 98:2)

Quellen und Nachweise

ORD-Eintrag
ord-0b074cf756224a2a97131207fa891ed8
Quelldatensatz
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06184236B2

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