Reaktion #1994274

Reaktionsgleichung

tri-n-butylamine

Tetrasodium diphosphate decahydrate

→

bis(tri-n-butylammonium) pyrophosphate

Lösungsmittel

EtOH

water

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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.

Quelle