Hexamethylphosphorous triamide → HCID 23414754, compound

HRID 259482Notes

Reaction equation

HRID 259482 reaction equation
[NH:1]1[CH2:10][CH2:9][CH2:8][NH:7][CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.CN(C)[P:13](N(C)C)N(C)C>C1(C)C=CC=CC=1>[N:1]12[P:13]3[N:4]([CH2:5][CH2:6][N:7]3[CH2:8][CH2:9][CH2:10]1)[CH2:3][CH2:2]2

Participants

4

Reactant 2

HCID 15355Hexamethylphosphorous triamideHCID 52483391,4,7-Triazecane

Product 1

HCID 23414754HCID 23414754, compoundYield 89%

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

A solution of 5.00 g of 1,4,7-triazacyclodecane and 5.70 g of hexamethylphosphorous triamide in 50 ml. of toluene is refluxed for 48 hours. The toluene is removed under reduced pressure, and the residue is distilled through a short-path column, to give 5.31 g (89%) of 1,4,7-triaza-11-phosphatricyclo[5.3.1.04,11 ] undecane as a clear, colorless liquid having a boiling point of 96°-98° C. at 0.70 mm. The product solidifies on standing at room temperature.

Workup

  1. customThe toluene is removed under reduced pressure
  2. distillationthe residue is distilled through a short-path column

Sources & evidence

ORD record
ord-3d1a6ff81f5d47468adb9d1add2ab010
Source dataset
uspto-grants-1977_07
Patent number
US04038312

Reaction notes

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