Propargylamine → HCID 178457409, Verbindung

HRID 27380

Reaktionsgleichung

Reaktionsgleichung von HRID 27380
[N+:1]([CH:4]=[C:5](SC)[NH:6][CH2:7][CH2:8][S:9][CH2:10][C:11]1[NH:15][CH:14]=[N:13][C:12]=1[CH3:16])([O-:3])=[O:2].[CH2:19]([NH2:22])[C:20]#[CH:21]>C(#N)C>[N+:1]([CH:4]=[C:5]([NH:22][CH2:19][C:20]#[CH:21])[NH:6][CH2:7][CH2:8][S:9][CH2:10][C:11]1[NH:15][CH:14]=[N:13][C:12]=1[CH3:16])([O-:3])=[O:2]

Komponenten

4

Edukt 2

HCID 239041PropargylamineHCID 178503826HCID 178503826, Verbindung

Produkt 1

HCID 178457409HCID 178457409, VerbindungAusbeute 87 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A mixture of 1-nitro-2-methylthio-2-{2-[(4-methyl-1H-imidazol-5-yl)methylthio]ethylamino}ethylene prepared according to Belgian Pat. No. 814,941 (4.0 g, 0.014 mole) and distilled propargylamine (7.74 g, 0.14 mole) in acetonitrile (60 ml) was stirred at reflux temperature under a positive pressure of nitrogen for 18 hours. The reaction mixture was cooled, evaporated to dryness and then triturated under 20 ml of isopropyl alcohol to give the title compound (3.58 g, 87%). Column chromatography on silica gel by gradient elution using methylene chloride-methanol gave a pure sample; mp 159°-160° dec.

Aufarbeitung

  1. customprepared
  2. temperatureat reflux temperature under a positive pressure of nitrogen for 18 hours
  3. temperatureThe reaction mixture was cooled
  4. customevaporated to dryness
  5. customtriturated under 20 ml of isopropyl alcohol

Quellen und Nachweise

ORD-Eintrag
ord-988f2b78e6134f9c8ad9f36d5d102635
Quelldatensatz
uspto-grants-1980_09
Patentnummer
US04221737

Verknüpfte Notizen

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