Water → HCID 54467132, Verbindung

HRID 568757Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 568757
C1(C(C2[C:14]([CH2:15][O:16][CH2:17][C:18]3[C:23](C4C(=CC=C(O)C=4)O)=[CH:22][CH:21]=[CH:20][CH:19]=3)=[CH:13][CH:12]=[CH:11][CH:10]=2)=CC(=CC=1)O)O.[CH3:32][CH:33]([O:40][C:41]1[CH:49]=[CH:48][C:44]([C:45](Cl)=[O:46])=[CH:43][CH:42]=1)[CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH3:39].[OH2:50]>N1C=CC=CC=1.C1(C)C=CC=CC=1>[CH2:17]([O:16][C:15]1[CH:10]=[CH:11][C:12]([O:46][C:45](=[O:50])[C:44]2[CH:48]=[CH:49][C:41]([O:40][CH:33]([CH3:32])[CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH3:39])=[CH:42][CH:43]=2)=[CH:13][CH:14]=1)[C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1

Komponenten

6

Edukt 3

HCID 962WaterHCID 13878422p-(1-Methyl-heptyloxy)benzoic acid chlorideHCID 1317110222-[2-[[2-(2,5-Dihydroxyphenyl)phenyl]methoxymethyl]phenyl]benzene-1,4-diol

Produkt 1

HCID 54467132HCID 54467132, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1049PyridineLösungsmittelHCID 1140TolueneLösungsmittel2×

Versuchsvorschrift

Hydroquinone monobenzyl ether (100.0 g, 0.50 mol) was dissolved in pyridine (600 ml), followed by dropwise adding to the solution, a solution of p-(1-methyl-heptyloxy)benzoic acid chloride (122.2 g, 0.45 mol) dissolved in toluene (600 ml), under ice cooling, agitating the mixture for 2 hours while keeping the temperature at about 50°-60° C., allowing it to stand overnight, thereafter adding toluene (3,000 ml) and water (2,000 ml), agitating the mixture, washing the toluene layer with 6N-HCl, then with 2N-NaOH aqueous solution and further with water until the wash water became neutral, distilling off toluene and recrystallizing the residue from ethanol to obtain p-(1-methyl-heptyloxy)-benzoic acid p-benzyloxyphenyl ester (121.0 g).

Aufarbeitung

  1. additionby dropwise adding to the solution
  2. customat about 50°-60° C.
  3. waitto stand overnight
  4. washwashing the toluene layer with 6N-HCl
  5. distillationdistilling off toluene
  6. customrecrystallizing the residue from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-788f1ac84ed14a249c81183e822d521e
Quelldatensatz
uspto-grants-1988_03
Patentnummer
US04729847

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