Dodecylamine → HCID 178443234, Verbindung

HRID 1462193Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1462193
[O:1]1[CH2:6][C:5](=O)[NH:4][C:3](=[O:8])[NH:2]1.[CH2:9]([NH2:21])[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH3:20].C[Si](C)(C)N[Si](C)(C)C>S([O-])([O-])(=O)=O.[NH4+].[NH4+].O1CCOCC1>[CH2:9]([NH:21][C:5]1[CH2:6][O:1][NH:2][C:3](=[O:8])[N:4]=1)[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH3:20]

Komponenten

6

Edukt 3

HCID 13583DodecylamineHCID 13838HexamethyldisilazaneHCID 642154HCID 642154, Verbindung

Produkt 1

HCID 178443234HCID 178443234, VerbindungAusbeute 88,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6097028Ammonium SulfateKatalysatorHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A solution of 1.16 g (0.010 mole) of 6H-1,2,4-oxadiazin-3,5(2H,4H)-dione, 5 mg of ammonium sulfate, 2.22 g (0.012 mole) of dodecylamine and 20 ml of hexamethyldisilazane in 40 ml of freshly distilled dry dioxane is refluxed for 17 hours. After cooling, the dioxane and hexamethyldisilazane are removed in vacuo and the syrupy residue is dried on a vacuum pump for 2 hours. The resulting semi-solid residue is triturated with 100 ml of petroleum ether and filtered to yield 2.5 g (88 percent) of 5-dodecylamino-6H-1,2,4-oxadiazin-3(2H)-one.

Aufarbeitung

  1. temperatureis refluxed for 17 hours
  2. temperatureAfter cooling
  3. customthe dioxane and hexamethyldisilazane are removed in vacuo
  4. customthe syrupy residue is dried on a vacuum pump for 2 hours
  5. customThe resulting semi-solid residue is triturated with 100 ml of petroleum ether
  6. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-9b28039e4f8a42f0b5600e820e311307
Quelldatensatz
uspto-grants-1984_07
Patentnummer
US04459403

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