Réaction #1994274

ord-03b70cdd0ea44649963edef03c08c64a

Équation de réaction

CCCCN(CCCC)CCCC
tri-n-butylamine
O.O.O.O.O.O.O.O.O.O.O=P([O-])([O-])OP(=O)([O-])[O-].[Na+].[Na+].[Na+].[Na+]
Tetrasodium diphosphate decahydrate
CCCC[NH+](CCCC)CCCC.CCCC[NH+](CCCC)CCCC.O=P([O-])([O-])OP(=O)(O)O
bis(tri-n-butylammonium) pyrophosphate

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    LavageThe column was eluted with water
  2. 2
    workup.ADDITIONThe eluent dropped directly into
  3. 3
    Températurea cooled (ice bath)
  4. 4
    LavageThe column was washed until the pH of the eluent
  5. 5
    Températureincreased to 6
  6. 6
    AutreThe aq. ethanol solution was evaporated to dryness
  7. 7
    workup.DISSOLUTIONThe residue was dissolved in DMF (6.7 ml)

Mode opératoire

Tetrasodium diphosphate decahydrate (1.5 g, 3.4 mmol) was dissolved in water (34 ml) and the solution was applied to a column of dowex in the H+ form. The column was eluted with water. The eluent dropped directly into a cooled (ice bath) and stirred solution of tri-n-butylamine (1.6 ml, 6.8 mmol) in EtOH (14 ml). The column was washed until the pH of the eluent increased to 6. The aq. ethanol solution was evaporated to dryness and then co-evaporated twice with ethanol and twice with anhydrous DMF. The residue was dissolved in DMF (6.7 ml). The pale yellow solution was stored over 4 Å molecular sieves.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08597881B2uspto-grants-2013_12