Sodium Iodide → HCID 178498267, Verbindung

HRID 726253

Reaktionsgleichung

Reaktionsgleichung von HRID 726253
[OH:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][CH:3]=1.Cl.Cl[CH2:14][CH2:15][C:16]1[N:17]=[CH:18][NH:19][CH:20]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>CN(C)C=O.C(Cl)(Cl)Cl.CO.C(Cl)(Cl)Cl>[C:6]([C:5]1[CH:4]=[CH:3][C:2]([O:1][CH2:14][CH2:15][C:16]2[N:17]=[CH:18][NH:19][CH:20]=2)=[CH:11][CH:10]=1)([O:8][CH3:9])=[O:7]

Komponenten

8

Edukt 4

HCID 5238Sodium IodideHCID 7456MethylparabenHCID 11430Potassium CarbonateHCID 1784785704-(2-chloroethyl)-1H-imidazole hydrochloride

Produkt 1

HCID 178498267HCID 178498267, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 6212ChloroformLösungsmittelHCID 6228DimethylformamideLösungsmittelHCID 21584188Chloroform methanolLösungsmittel

Versuchsvorschrift

228 mg (1.5 mmol) of methyl 4-hydroxybenzoate, 251 mg (1.5 mmol) of 4-[2-chloroethyl]-1H-imidazole hydrochloride, 500 mg (3.6 mmol) of potassium carbonate and sodium iodide (catalyst) are stirred at 80° C. for 3 days in 5 ml of dimethylformamide. The reaction mixture is cooled and filtered and the filtrate is evaporated under reduced pressure to give an oily residue which is subjected to column chromatography (using, as first eluent, chloroform and, as second eluent, a 95/5 chloroform/methanol mixture). The product is purified by preparative high performance liquid chromatography and crystallized from water; M.p.: 116°-118° C.

Aufarbeitung

  1. temperatureThe reaction mixture is cooled
  2. filtrationfiltered
  3. customthe filtrate is evaporated under reduced pressure
  4. customto give an oily residue which
  5. customThe product is purified by preparative high performance liquid chromatography
  6. customcrystallized from water

Quellen und Nachweise

ORD-Eintrag
ord-de1c05e228e64aefb3975d839f8ae725
Quelldatensatz
uspto-grants-1998_01
Patentnummer
US05708171

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