Dimethyl Sulfoxide → HCID 70539474, Verbindung

HRID 1065477Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1065477
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH:9]([NH:11][CH2:12][CH2:13][CH:14]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH3:10])=[CH:4][CH:3]=1.CS(C)=[O:29].[OH-:31].[Na+].[C:33]([C:37]1[CH:44]=[CH:43][C:40]([CH2:41]Cl)=[CH:39][CH:38]=1)([CH3:36])([CH3:35])[CH3:34].[OH2:45]>>[C:2]([OH:1])(=[O:29])/[CH:7]=[CH:6]\[C:5]([OH:45])=[O:31].[C:33]([C:37]1[CH:38]=[CH:39][C:40]([CH2:41][O:1][C:2]2[CH:3]=[CH:4][C:5]([CH2:8][CH:9]([NH:11][CH2:12][CH2:13][CH:14]([C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=3)[C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH3:10])=[CH:6][CH:7]=2)=[CH:43][CH:44]=1)([CH3:36])([CH3:34])[CH3:35]

Komponenten

6

Edukt 5

HCID 679Dimethyl SulfoxideHCID 962WaterHCID 14798Sodium HydroxideHCID 88198Benzene, 1-(chloromethyl)-4-(1,1-dimethylethyl)-HCID 130652814-{2-[(3,3-Diphenylpropyl)amino]propyl}phenol

Produkt 1

HCID 70539474HCID 70539474, Verbindung

Versuchsvorschrift

The mixture of 18.3 g of 1-(4-hydroxyphenyl)-2-(3,3-diphenylpropylamino)-propane, 100 ml of dimethylsulfoxide and 5.29 ml of 10 N-aqueous sodium hydroxide is stirred at room temperature for one hour, combined with 9.66 g of 4-t-butylbenzyl chloride and stirred 18 hours longer. It is poured into 1,000 ml of water, extracted twice with 500 ml of methylene chloride, the extract dried and evaporated at about 60°. The residue is taken up in isopropanol, the solution acidified with 5% isopropanolic maleic acid, the precipitate collected and recrystallized from isopropanol-diethyl ether, to yield the 1-[4-(4-t-butylbenzyloxy)-phenyl]-2-(3,3-diphenylpropylamino)-propane maleate melting at 132°-134°.

Aufarbeitung

  1. stirringstirred 18 hours longer
  2. extractionextracted twice with 500 ml of methylene chloride
  3. customthe extract dried
  4. customevaporated at about 60°
  5. customthe precipitate collected
  6. customrecrystallized from isopropanol-diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-846945c261a44b5bb2d515c2831917e0
Quelldatensatz
uspto-grants-1982_05
Patentnummer
US04329367

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