Diethyl Ether → HCID 14424276, Verbindung

HRID 414222Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 414222
[Br:1][CH2:2][C:3]([C:5]1[S:6][C:7]([CH3:10])=[CH:8][CH:9]=1)=[O:4].[CH2:11]1[N:16]2[CH2:17][N:18]3[CH2:20][N:14]([CH2:15]2)[CH2:13][N:12]1[CH2:19]3.C(OCC)C>C(Cl)(Cl)Cl.C(Cl)Cl>[Br-:1].[O:4]=[C:3]([C:5]1[S:6][C:7]([CH3:10])=[CH:8][CH:9]=1)[CH2:2][N+:12]12[CH2:13][N:14]3[CH2:20][N:18]([CH2:17][N:16]([CH2:15]3)[CH2:11]1)[CH2:19]2

Komponenten

6

Edukt 3

HCID 3283Diethyl EtherHCID 4101HexamethylenetetramineHCID 122897372-Bromo-1-(5-methyl-2-thienyl)ethanone

Produkt 1

HCID 14424276HCID 14424276, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6212ChloroformLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of 2-bromo-1-(5-methylthien-2-yl)ethanone (30.0 g of the aforesaid dark liquid) and hexamethylene tetramine (21.0 g, 0.15 mole) in chloroform (500 ml) was stirred at room temperature for three days. The solvent was removed from the reaction mixture by evaporation under reduced pressure, leaving a dark residue. This residue was stirred in warm methylene chloride. Diethyl ether was added slowly to the mixture, causing a solid to precipitate. After being cooled for several hours, the solid was collected by filtration. The filter cake was rinsed with diethyl ether and was dried under reduced pressure yielding 43.1 g of 1-[2-oxo-2-(5-methylthienyl)ethyl]-3,5,7-triaza-1-azoniatricyclo-[3,3,1,13,7 ]decane bromide (mp 141° C. dec).

Aufarbeitung

  1. customThe solvent was removed from the reaction mixture by evaporation under reduced pressure
  2. customleaving a dark residue
  3. customto precipitate
  4. temperatureAfter being cooled for several hours
  5. filtrationthe solid was collected by filtration
  6. washThe filter cake was rinsed with diethyl ether
  7. customwas dried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-51558efb2e724ccc8c8f6c59ae0ef28c
Quelldatensatz
uspto-grants-1988_12
Patentnummer
US04791124

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