Butylamine → HCID 178448892, Verbindung

HRID 1462196Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1462196
[O:1]1[CH2:6][C:5](=O)[NH:4][C:3](=[O:8])[NH:2]1.[CH2:9]([NH2:13])[CH2:10][CH2:11][CH3:12].C[Si](C)(C)N[Si](C)(C)C>S([O-])([O-])(=O)=O.[NH4+].[NH4+].O1CCOCC1>[CH2:9]([NH:13][C:5]1[CH2:6][O:1][NH:2][C:3](=[O:8])[N:4]=1)[CH2:10][CH2:11][CH3:12]

Komponenten

6

Edukt 3

HCID 8007ButylamineHCID 13838HexamethyldisilazaneHCID 642154HCID 642154, Verbindung

Produkt 1

HCID 178448892HCID 178448892, VerbindungAusbeute 87 %

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, 0.88 g (0.012 mole) of n-butylamine and 20 ml hexamethyldisilazane in 40 ml freshly distilled dry dioxane is refluxed for 17 hours. After cooling to room temperature, 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 1.02 g (87 percent) of 5-butylamino-6H-1,2,4-oxadiazin-3(2H)-one.

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-7613d32658ee408c9d3d805ce159a2c4
Quelldatensatz
uspto-grants-1984_07
Patentnummer
US04459403

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