Dimethylamine → Hexahydro-1H,4H,7H-3a,6a,9a-triaza-9b-phosphaphenalene

HRID 1973177

Reaktionsgleichung

Reaktionsgleichung von HRID 1973177
[NH:1]1[CH2:12][CH2:11][CH2:10][NH:9][CH2:8][CH2:7][CH2:6][NH:5][CH2:4][CH2:3][CH2:2]1.CNC.CN(C)[P:18](N(C)C)N(C)C>>[N:1]12[P:18]3[N:9]([CH2:8][CH2:7][CH2:6][N:5]3[CH2:4][CH2:3][CH2:2]1)[CH2:10][CH2:11][CH2:12]2

Komponenten

4

Edukt 3

HCID 674DimethylamineHCID 15355Hexamethylphosphorous triamideHCID 4707781,5,9-Triazacyclododecane

Produkt 1

HCID 333382Hexahydro-1H,4H,7H-3a,6a,9a-triaza-9b-phosphaphenaleneAusbeute 76 %

Versuchsvorschrift

A mixture of 4.20 g of 1,5,9-triazacyclododecane and 4.00 g of hexamethylphosphorous triamide is heated at 100° C for about six hours, by which time evolution of dimethylamine is complete. Distillation under reduced pressure gives 3.70 g (76%) of 1,5,9-triaza-13-phosphatricyclo-[7.3.1.05,13 ]tridecane as a clear, colorless liquid which boils at 104°-135° C at 0.60 mm. The product solidifies at room temperature. Its infrared absorption spectrum (neat) shows absorptions at 3.5, 6.85, 7.01, 7.52, 7.73, 8.00, 8.27, 8.66, 8.90, 9.02, 9.36, 9.56, 10.27, 10.89, 11.42, 11.73, 11.97 and 14.7 μ. The mass spectrum shows an M+ ion at 199; measured mass, 199.1264; calc'd, 199.1238.

Aufarbeitung

  1. distillationDistillation under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-ea1c9badf517452ebff33d295102bd0d
Quelldatensatz
uspto-grants-1976_12
Patentnummer
US03996276

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