Pyridine → HCID 13627682, Verbindung

HRID 1789086Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1789086
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][CH3:16])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.[CH2:17]([O:22][C:23]1[CH:28]=[CH:27][C:26]([CH2:29][CH2:30][C:31](Cl)=[O:32])=[CH:25][CH:24]=1)[CH2:18][CH2:19][CH2:20][CH3:21].N1C=CC=C[CH:35]=1>O>[CH3:35][CH:30]([CH2:29][C:26]1[CH:27]=[CH:28][C:23]([O:22][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])=[CH:24][CH:25]=1)[C:31]([O:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][CH3:16])=[CH:10][CH:9]=2)=[CH:6][CH:7]=1)=[O:32]

Komponenten

5

Edukt 3

HCID 1049PyridineHCID 136276804-(4-n-Propylphenyl)phenolHCID 53826862HCID 53826862, Verbindung

Produkt 1

HCID 13627682HCID 13627682, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

4-Hydroxy-4'-propylbiphenyl (2.5 g, 0.012 mol) was dissolved in pyridine (10 ml) and to the solution was added β-(4-pentyloxyphenyl)propionic acid chloride (2.5 g, 0.01 mol) with sufficient shaking, followed by allowing the resulting reaction solution to stand overnight, pouring it in water (100 ml), extracting the resulting oily material with toluene (100 ml), washing the toluene layer with 6N-HCl, then with 2N-NaOH and further with water till the washing water became neutral, filtering, distilling off toluene under reduced pressure, and recrystallizing residual crystals from ethanol to obtain the objective 4'-propyl-4-biphenylyl α-methyl-β-(4-pentyloxyphenyl)propionate. m.p. 84.0°-84.5° C. N-I point 46.0° C. (extrapolated value).

Aufarbeitung

  1. customthe resulting reaction solution
  2. extractionextracting the resulting oily material with toluene (100 ml)
  3. washwashing the toluene layer with 6N-HCl
  4. filtrationfiltering
  5. distillationdistilling off toluene under reduced pressure
  6. customrecrystallizing residual crystals from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-149cf621368447ca9478e75c0d11594b
Quelldatensatz
uspto-grants-1987_08
Patentnummer
US04686305

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