Реакция #357935

ord-16e1e9eee7ef496084f3b545b516fbda

Реагенты

Нет

Растворители

Условия реакции

Температура
10°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеlower, whereupon a white solid precipitated
  2. 2
    ФильтрацияThe white solid was collected by filtration
  3. 3
    Промывкаwashed with water
  4. 4
    workup.ADDITIONTo the filtrate was added 300 g of methanol
  5. 5
    Фильтрацияthe thus precipitated white solid was collected by filtration
  6. 6
    Промывкаwashed with methanol and water
  7. 7
    ДругоеThe combined white solid was dried

Методика

In 300 g of water was dispersed 0.5 mol of sodium pyrophosphate. The dispersion was cooled to 10° C., and 1 mol of hydrochloric acid was added thereto. To the dispersion was added 0.5 mol of piperazine (purity: 97%) dissolved in 800 g of water at 20° C. or lower, whereupon a white solid precipitated. The reaction system was stirred at 10° C. for 3 hours. The white solid was collected by filtration and washed with water. To the filtrate was added 300 g of methanol, and the thus precipitated white solid was collected by filtration and washed with methanol and water. The combined white solid was dried to give 0.23 mol of piperazine pyrophosphate as a white powder.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07449577B2uspto-grants-2008_11