Ethanol → 1,3-Dimethyl-2-imidazolinone Ethanol

HRID 464234

Reaktionsgleichung

Reaktionsgleichung von HRID 464234
[Cl-].[Li+].[CH3:3][N:4]1[CH2:8][CH2:7][N:6]([CH3:9])[C:5]1=O.[CH2:11]([OH:13])[CH3:12]>C[C@@H]([C@@H]1[C@@]2(C)CC[C@@H]3[C@@]4(C)CC[C@@H](O)C[C@H]4CC(=O)[C@H]3[C@@H]2CC1)CCC(O)=O>[CH3:3][N:4]1[CH2:5][N:6]([CH3:9])[C:7](=[O:13])[CH2:8]1.[CH2:11]([OH:13])[CH3:12]

Komponenten

5

Edukt 3

HCID 702EthanolHCID 66611,3-Dimethyl-2-imidazolidinoneHCID 433294Lithium Chloride

Produkt 1

HCID 704730901,3-Dimethyl-2-imidazolinone Ethanol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 4442627-Ketolithocholic acidLösungsmittel

Versuchsvorschrift

In an undivided flow-through cell with ruthenized titatium anode and cathode, 1.95 g of 7-ketolithocholic acid was dissolved in an electrolyte made from 0.65 g of lithium chloride, 60 mL of 1,3-dimethyl 2-imidazolidinone and 200 mL of absolute ethanol. The solution in both the cell and the reservoir was kept under nitrogen. Initially, current of up to 4 amperes were passed through the cell but polarization occurred and the current had to be reduced to 400 ma. Electrolysis was continued until 97 coulombs had been delivered. The solvent was removed under high vacuum, and the residue dissolved in 2N sodium hydroxide. The product was precipitated by adding this alkaline solution dropwise to acidic (pH 2.0) water. The recovery was 76.9%. The percent reduction was 36.8. The ratio of ursodeoxycholic acid to chenodeoxycholic acid was 1.45.

Aufarbeitung

  1. customThe solvent was removed under high vacuum
  2. dissolutionthe residue dissolved in 2N sodium hydroxide
  3. customThe product was precipitated
  4. additionby adding this alkaline solution dropwise to acidic (pH 2.0) water

Quellen und Nachweise

ORD-Eintrag
ord-0d10ef6b44a54d52871ca9343fea3dbf
Quelldatensatz
uspto-grants-1985_10
Patentnummer
US04547271

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