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

HRID 259483

Reaktionsgleichung

Reaktionsgleichung von HRID 259483
[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 6 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-f85731e5adc4449cbc7c46040f22e5c5
Quelldatensatz
uspto-grants-1977_07
Patentnummer
US04038312

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