Methanol → 1-Methyl-3-phenoxypropyldiethylamine

HRID 464811Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 464811
CO.S(C1C=CC(C)=CC=1)(O[CH:7]([CH2:9][CH2:10][O:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[CH3:8])(=O)=O.[CH2:25]([NH:27][CH2:28][CH3:29])[CH3:26].C(OCC)C>C(Cl)(Cl)Cl>[CH3:8][CH:7]([N:27]([CH2:28][CH3:29])[CH2:25][CH3:26])[CH2:9][CH2:10][O:11][C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1

Komponenten

6

Edukt 4

HCID 887MethanolHCID 3283Diethyl EtherHCID 8021DiethylamineHCID 133267624-Phenoxy-2-butyl tosylate

Produkt 1

HCID 135201021-Methyl-3-phenoxypropyldiethylamineAusbeute 77 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

To 60 ml of absolute methyl alcohol were added 10 g of 4-phenoxy-2-butyl tosylate and 9.62 g of diethylamine. The mixture was reacted in a sealed tube for one hour at 125° C. After the reaction solution was condensed under reduced pressure, 100 ml of diethyl ether was added into the solution and the solution was separated with 20% aqueous sodium hydroxide solution. The ether layer was dried with anhydrous sodium sulfate, and the ether was removed under reduced pressure therefrom. The residue thus obtained was subjected to alumina-column chromatography using chloroform as the solvent to give 5.32 g of 1-methyl-3-phenoxypropyldiethylamine in a yield of 77%.

Aufarbeitung

  1. customThe mixture was reacted in a sealed tube for one hour at 125° C
  2. additionwas added into the solution
  3. customthe solution was separated with 20% aqueous sodium hydroxide solution
  4. dry with materialThe ether layer was dried with anhydrous sodium sulfate
  5. customthe ether was removed under reduced pressure
  6. customThe residue thus obtained

Quellen und Nachweise

ORD-Eintrag
ord-c0f668ad448447cbba3fa49b9ba6c15e
Quelldatensatz
uspto-grants-1985_10
Patentnummer
US04549023

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