Iodine → HCID 178439117, Verbindung

HRID 342352

Reaktionsgleichung

Reaktionsgleichung von HRID 342352
S(=O)(=O)(O)O.[CH2:6]([C:9]1[CH:14]=[CH:13][C:12]([C@H:15]2[CH2:20][CH2:19][C@H:18]([CH2:21][CH2:22][C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[CH2:17][CH2:16]2)=[CH:11][CH:10]=1)[CH2:7][CH3:8].II.[I:31](O)(=O)=O>O.C(Cl)(Cl)(Cl)Cl.C(O)(=O)C>[CH2:6]([C:9]1[CH:14]=[CH:13][C:12]([C@H:15]2[CH2:16][CH2:17][C@H:18]([CH2:21][CH2:22][C:23]3[CH:24]=[CH:25][C:26]([I:31])=[CH:27][CH:28]=3)[CH2:19][CH2:20]2)=[CH:11][CH:10]=1)[CH2:7][CH3:8]

Komponenten

8

Edukt 4

HCID 807IodineHCID 1118Sulfuric AcidHCID 24345Iodic acidHCID 178439111HCID 178439111, Verbindung

Produkt 1

HCID 178439117HCID 178439117, VerbindungAusbeute 118 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 176Acetic AcidLösungsmittelHCID 962WaterLösungsmittelHCID 5943Carbon TetrachlorideLösungsmittel

Versuchsvorschrift

To a liquid mixture comprising 50 ml of acetic acid, 5 ml of carbon tetrachloride, 5 ml of concentrated sulfuric acid, and 10 ml of water, were added 5.8 g of the (2-(trans-4-(4-n-propylphenyl)cyclohexyl)ethyl)benzene mentioned above, 2.4 g of iodine, and 2 g of iodic acid, and they were stirred under a reflux for 2 hours. After cooled, the mixture was washed with a saturated aqueous solution of sodium thiosulfate. Organic layer was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under a reduced pressure to obtain a yellow-brown oily product. This product was purified by a column chromatography over an alumina by using heptane as an eluent, and further recrystallized from heptane to obtain 5.8 g of 4-(2-(trans-4-(4-n-propylphenyl)cyclohexyl)ethyl)iodobenzene.

Aufarbeitung

  1. temperaturea reflux for 2 hours
  2. temperatureAfter cooled
  3. washthe mixture was washed with a saturated aqueous solution of sodium thiosulfate
  4. washOrganic layer was washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under a reduced pressure
  7. customto obtain a yellow-brown oily product
  8. customThis product was purified by a column chromatography over an alumina
  9. customfurther recrystallized from heptane

Quellen und Nachweise

ORD-Eintrag
ord-6242de626c4144a08f1480a88e791be2
Quelldatensatz
uspto-grants-1999_01
Patentnummer
US05858275

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