反応 #1994274

反応方程式

tri-n-butylamine

Tetrasodium diphosphate decahydrate

→

bis(tri-n-butylammonium) pyrophosphate

溶媒

EtOH

water

反応条件

後処理

1. 1
   洗浄The column was eluted with water
2. 2
   workup.ADDITIONThe eluent dropped directly into
3. 3
   温度a cooled (ice bath)
4. 4
   洗浄The column was washed until the pH of the eluent
5. 5
   温度increased to 6
6. 6
   その他The aq. ethanol solution was evaporated to dryness
7. 7
   workup.DISSOLUTIONThe residue was dissolved in DMF (6.7 ml)

実験手順

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.

出典