Hexamethylphosphorous triamide → HCID 54097162, compound

HRID 259481Notes

Reaction equation

HRID 259481 reaction equation
[O: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>C1(C)C=CC=CC=1>[N:10]12[P:15]3[N:7]([CH2:6][CH2:5][N:4]3[CH2:3][CH2:2][O:1][CH2:12][CH2:11]1)[CH2:8][CH2:9]2

Participants

4

Reactant 2

HCID 15355Hexamethylphosphorous triamideHCID 7715961-oxa-4,7,10-triazacyclododecane

Product 1

HCID 54097162HCID 54097162, compoundYield 102.5%

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

A solution of 2.50 g of 1-oxa-4,7,10-triazacyclododecane and 2.35 g of hexamethylphosphorous triamide in 25 ml of toluene is refluxed for 40 hours. It is then concentrated to dryness in a rotary evaporator, to give 2.97 g (100%) of 10-oxa-1,4,7-triaza-13-phosphatricyclo[5.5.1.04,13 ]tridecane as a brittle, white solid. Sublimation at 80° C. (0.007 mm) gives 2.08 g of white crystals having a melting point of 68°-70° C.

Workup

  1. concentrationIt is then concentrated to dryness in a rotary evaporator

Sources & evidence

ORD record
ord-07efe5190c0e4d55be7ecfa3b7bbe826
Source dataset
uspto-grants-1977_07
Patent number
US04038312

Reaction notes

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