反应详情

Tetrasodium diphosphate decahydrate (2.23 g, 5 mmol) was dissolved in water (50 mL), the solution was applied to a column of Dowex 50WX8 (100 mL) in the pyridinium form, and the column was washed with 300 mL water-methanol (1:1). The eluate was directly dropped into a cooled (ice water) and stirred solution of tri-n-butylamine (2.38 mL, 10 mmol) in methanol. The solution was evaporated to dryness and re-evaporated twice with methanol and finally with anhydrous DMF (30 mL) on an oil pump.

1. washthe column was washed with 300 mL water-methanol (1:1)
2. additionThe eluate was directly dropped into
3. temperaturea cooled (ice water)
4. customThe solution was evaporated to dryness
5. customre-evaporated twice with methanol and finally with anhydrous DMF (30 mL) on an oil pump