Hydrogen Bromide → HCID 12660548, compound

HRID 1732844Notes

Reaction equation

HRID 1732844 reaction equation
C([NH:5][CH2:6][P:7](=[O:20])([CH2:14][NH:15]C(OC)=O)[CH2:8][NH:9]C(OC)=O)(OC)=O.[BrH:21]>>[BrH:21].[BrH:21].[BrH:21].[NH2:5][CH2:6][P:7](=[O:20])([CH2:14][NH2:15])[CH2:8][NH2:9]

Participants

3

Reactant 2

HCID 260Hydrogen BromideHCID 326843methyl N-[bis[(methoxycarbonylamino)methyl]phosphorylmethyl]carbamate

Product 1

HCID 12660548HCID 12660548, compoundYield 49.9%

Procedure

A solution of 31.12 g (0.1 mol) of tris(N-carbomethoxyaminomethyl)phosphine oxide in 100 ml of constant-boiling (47-49%) hydrobromic acid was heated to reflux with constant stirring. Within a few minutes, solids started to separate. The mixture was heated at reflux for one hour, cooled, and filtered. The filter cake, rinsed with ethanol and air-dried, afforded 18.95 g (49.9% yield) of tris(aminomethyl)phosphine oxide trihydrobromide as a white, crystalline solid, dec. 233° C. with reddening. Another 2.60 g (6.8% yield) was recovered from the filtrate after heating at reflux an additional hour.

Workup

  1. temperatureto reflux with constant stirring
  2. waitWithin a few minutes
  3. customto separate
  4. temperatureThe mixture was heated
  5. temperatureat reflux for one hour
  6. temperaturecooled
  7. filtrationfiltered
  8. washThe filter cake, rinsed with ethanol
  9. customair-dried

Sources & evidence

ORD record
ord-de93ce0e43f6418e98af49ceafef0bf9
Source dataset
uspto-grants-1980_12
Patent number
US04239701

Reaction notes

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