Potassium Persulfate → HCID 10707356, Verbindung

HRID 1018661Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1018661
[CH:1]1([CH2:7][O:8][C:9]2[CH:10]=[CH:11][C:12]3[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][C:13]=3[CH:19]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.S(OOS([O-])(=O)=O)([O-])(=O)=[O:21].[K+].[K+].CC#N.O>O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Cu+2]>[CH:1]1([CH2:7][O:8][C:9]2[CH:10]=[CH:11][C:12]3[C:18](=[O:21])[CH2:17][CH2:16][CH2:15][CH2:14][C:13]=3[CH:19]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

Komponenten

6

Edukt 3

HCID 24412Potassium PersulfateHCID 18373917Acetonitrile--water (1/1)HCID 18401890HCID 18401890, Verbindung

Produkt 1

HCID 10707356HCID 10707356, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 24463Copper sulfate pentahydrateKatalysatorHCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 2-cyclohexylmethoxy-6,7,8,9-tetrahydro-5H-benzocycloheptene (0.50 g, 1.94 mmol), potassium persulfate (1.57 g, 5.82 mmol), copper(II) sulfate pentahydrate (0.48 g, 1.94 mmol) and CH3CN/H2O (1:1, 13 mL) were heated at reflux for 45 min. After cooling the mixture was diluted with water and extracted with EtOAc. The combined extracts were washed with water, dried over magnesium sulfate, concentrated, and chomatographed over silica gel (20% EtOAc/hexane) to a white solid (0.46 g, 87%). MS [M+H]+ 273, m.p. 86-88° C.

Aufarbeitung

  1. temperaturewere heated
  2. temperatureat reflux for 45 min
  3. temperatureAfter cooling the mixture
  4. extractionextracted with EtOAc
  5. washThe combined extracts were washed with water
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-98b3c83bdfca401090720dcf112d2839
Quelldatensatz
uspto-grants-2002_11
Patentnummer
US06482852B2

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