Water → Theofibrate

HRID 1287238

Reaktionsgleichung

Reaktionsgleichung von HRID 1287238
[Cl:1][C:2]1[CH:14]=[CH:13][C:5]([O:6][C:7]([CH3:12])([CH3:11])[C:8]([OH:10])=[O:9])=[CH:4][CH:3]=1.O[CH2:16][CH2:17][N:18]1[C:27]2[C:26](=[O:28])[N:24]([CH3:25])[C:23](=[O:29])[N:22]([CH3:30])[C:21]=2[N:20]=[CH:19]1.O.C(=O)(O)[O-].[Na+]>C1(C)C(C)=CC=CC=1.C1(C)C=CC(S(O)(=O)=O)=CC=1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:6][C:7]([CH3:12])([CH3:11])[C:8]([O:10][CH2:16][CH2:17][N:18]2[C:27]3[C:26](=[O:28])[N:24]([CH3:25])[C:23](=[O:29])[N:22]([CH3:30])[C:21]=3[N:20]=[CH:19]2)=[O:9])=[CH:13][CH:14]=1

Komponenten

7

Edukt 4

HCID 962WaterHCID 1892EtofyllineHCID 2797Clofibric AcidHCID 516892Sodium Bicarbonate

Produkt 1

HCID 41109TheofibrateAusbeute 55,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6101p-Toluenesulfonic acidKatalysatorHCID 7237O-XyleneLösungsmittel

Versuchsvorschrift

107.3 g (0.5 mol) 2-(p-chlorophenoxy) isobutyric acid and 56.0 g (0.25 mol) 7-hydroxyethyltheophylline were suspended together in 250 ml xylene and heated for 15 hours in a water separator after addition of 1.5 g p-toluenesulfonic acid. The solution was next agitated with dilute sodium bicarbonate solution (0.5 mol NaHCO3), waterwashed and evaporated in a rotary evaporator. The residue was crystallized from isopropanol, yielding 58.0 g (55% yield) 1-(7-theophyllinyl)-2-ethyl [2-(p-chlorophenoxy)-isobutyrate] with a melting point 131°-132°C.

Aufarbeitung

  1. customwaterwashed and evaporated in a rotary evaporator
  2. customThe residue was crystallized from isopropanol

Quellen und Nachweise

ORD-Eintrag
ord-5842ddc15eb14601bf44c55cda34357f
Quelldatensatz
uspto-grants-1976_10
Patentnummer
US03984413

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