Hexamethylphosphorous triamide → 1,4,7,10Tetraaza-13-phosphatricyclo[5.5.1.04,13]tridecane

Reaction equation

[NH:1]1[CH2:12][CH2:11][NH:10][CH2:9][CH2:8][NH:7][CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.CN(C)[P:15](N(C)C)N(C)C>>[N:1]12[P:15]3[N:4]([CH2:5][CH2:6][N:7]3[CH2:8][CH2:9][NH:10][CH2:11][CH2:12]1)[CH2:3][CH2:2]2

Participants

Reactant 2

HCID 15355Hexamethylphosphorous triamide

HCID 649631,4,7,10-Tetraazacyclododecane

Product 1

HCID 536936111,4,7,10Tetraaza-13-phosphatricyclo[5.5.1.04,13]tridecane

Procedure

1,4,7,10Tetraaza-13-phosphatricyclo[5.5.1.04,13 ]tridecane is prepared in the absence of a solvent by heating 5.0 g of 1,4,7,10-tetraazacyclododecane and 4.7 g of hexamethylphosphorous triamide together at about 75° C for between two and three hours and subliming the crude product at 75° C. at 0.4 mm. The yield is 5.3 g (92%) of product melting at 106°-108° C.

Workup

customat 75° C.

Sources & evidence

ORD record: ord-e669fa70a9c344e2aa49e6478311a198
Source dataset: uspto-grants-1977_07
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US04038312

Reaction notes

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