Dimethyl Sulfoxide → HCID 70620955, Verbindung

HRID 2420470Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2420470
[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.[OH-:27].[Na+].CS(C)=[O:31].[CH3:33][C:34]1[CH:35]=[CH:36][C:37]([CH2:40]Cl)=[N:38][CH:39]=1.[OH2:42]>>[C:2]([OH:1])(=[O:31])/[CH:7]=[CH:6]\[C:5]([OH:42])=[O:27].[CH3:33][C:34]1[CH:35]=[CH:36][C:37]([CH2:40][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)=[N:38][CH:39]=1

Komponenten

6

Edukt 5

HCID 679Dimethyl SulfoxideHCID 962WaterHCID 14798Sodium HydroxideHCID 5880562-(Chloromethyl)-5-methylpyridineHCID 130652814-{2-[(3,3-Diphenylpropyl)amino]propyl}phenol

Produkt 1

HCID 70620955HCID 70620955, Verbindung

Versuchsvorschrift

The mixture of 21.76 g of dl-1-(4-hydroxyphenyl)-2-(3,3-diphenylpropylamino)-propane, 6.3 ml of 10 N aqueous sodium hydroxide and 100 ml of dimethylsulphoxide is stirred at 60° for 2 hours, whereupon 8.91 g of 5-methyl-2-pyridylmethyl chloride are added. The whole is stirred at ambient temperature for 24 hours, diluted with 400 ml of water and extracted with methylene chloride. The extract is dried, evaporated, the residual oil taken up in isopropanol and the solution acidified with maleic acid in isopropanol until the pH of 5 is reached, to yield the dl-1-[4-(5-methyl-2-pyridylmethoxy)-phenyl]-2-(3,3-diphenylpropylamino)propane maleate, melting at 155°-157°.

Aufarbeitung

  1. additionare added
  2. extractionextracted with methylene chloride
  3. customThe extract is dried
  4. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-d344c61602c945d581a4f0b1d3be333a
Quelldatensatz
uspto-grants-1978_08
Patentnummer
US04110457

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