Реакция #94101

ord-4f353ea2a7a64395b4c6d4bfd0269ea2

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеA deep blue solution was formed
  2. 2
    ДругоеThis solution, when evaporated to dryness
  3. 3
    Другоеgave a deep blue, semicrystalline solid
  4. 4
    Экстракцияthe lithium chloride was extracted with 50 milliliters of dry methanol, five times, at 35° C
  5. 5
    Другоеbehind was evacuated
  6. 6
    Другоеto remove methanol
  7. 7
    Другоеto crystallize the salt from water-organic solvent systems
  8. 8
    workup.ADDITIONapparently due to the extremely hygroscopic nature of the salt and the high negative charge on the ionized molecule
  9. 9
    Другоеthe solid obtained

Методика

10 millimoles of lithium citrate were dissolved in 10 milliliters of water. To this solution, 10 millimoles of cupric chloride (CuCl2.2H2O) were added gradually with stirring. A deep blue solution was formed. This was neutralized to a pH of about 7 with 10 millimoles of lithium hydroxide (LiOH.H2O). This solution, when evaporated to dryness, gave a deep blue, semicrystalline solid. This solid was ground to a fine powder and the lithium chloride was extracted with 50 milliliters of dry methanol, five times, at 35° C. The blue solid which remained behind was evacuated to remove methanol and desiccated. An attempt was made to crystallize the salt from water-organic solvent systems, but apparently due to the extremely hygroscopic nature of the salt and the high negative charge on the ionized molecule, the solid obtained was microcrystalline to amorphous. The following formula is proposed for the 1:1 complex of copper and citrate based on elucidation of the structure and analyses described hereinafter.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04129509uspto-grants-1978_12