Reacción #1994274

Ecuación de reacción

tri-n-butylamine

Tetrasodium diphosphate decahydrate

→

bis(tri-n-butylammonium) pyrophosphate

Disolventes

EtOH

water

Condiciones de reacción

Tratamiento posterior

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

Procedimiento

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.

Fuente