Formaldehyde → 2-Thia-1,3,5-triaza-7-phosphaadamantane 2,2-dioxide

HRID 1579946Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1579946
O[CH2:2][P:3]([CH2:6]O)[CH2:4]O.C=O.[S:10]([NH2:14])([NH2:13])(=[O:12])=[O:11].[CH2:15]1N2CN3CN(C2)[CH2:17][N:16]1C3>O>[N:13]12[CH2:17][N:16]3[CH2:2][P:3]([CH2:6][N:14]([CH2:15]3)[S:10]1(=[O:12])=[O:11])[CH2:4]2

Komponenten

6

Edukt 4

HCID 712FormaldehydeHCID 4101HexamethylenetetramineHCID 76001Tris(Hydroxymethyl)PhosphineHCID 82267Sulfamide

Produkt 1

HCID 218292932-Thia-1,3,5-triaza-7-phosphaadamantane 2,2-dioxideAusbeute 66 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Tris(hydroxymethyl)phosphine (3.9 g, 80%, 0.025 moles) was dissolved in formalin (20 ml, 40%, 0.267 moles) and water (20 ml). Sulfamide (2.4 g, 0.025 mole) and hexamethylenetetramine (3.5 g, 0.025 mole) were added together and dissolved in the solution at room temperature. The solution heated up slightly and over the next twenty-four hours a precipitate formed. Filtration, dissolution of the solid in 4 successive 30 ml acetone washes and evaporation of the acetone yielded 3.42 g of crude 2-thia-1,3,5-triaza-7-phosphaadamantane 2,2-dioxide (66% yield) [mp 274°-5° (water)].

Aufarbeitung

  1. dissolutiondissolved in the solution at room temperature
  2. temperatureThe solution heated up slightly and over the next twenty-four hours a precipitate
  3. customformed
  4. filtrationFiltration, dissolution of the solid
  5. customin 4 successive 30 ml acetone washes and evaporation of the acetone

Quellen und Nachweise

ORD-Eintrag
ord-073edc8f41924737b6357787a100ba9b
Quelldatensatz
uspto-grants-1976_01
Patentnummer
US03932390

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