반응 #1994274

반응 방정식

tri-n-butylamine

Tetrasodium diphosphate decahydrate

→

bis(tri-n-butylammonium) pyrophosphate

용매

EtOH

water

반응 조건

후처리

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

실험 절차

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.

출처