Реакция #1994274

Уравнение реакции

tri-n-butylamine

Tetrasodium diphosphate decahydrate

→

bis(tri-n-butylammonium) pyrophosphate

Растворители

EtOH

water

Условия реакции

Обработка

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

Методика

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.

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