Chromium(3+) trichloride hexahydrate → Chromium(III) picolinate

HRID 1941064

Reaktionsgleichung

Reaktionsgleichung von HRID 1941064
O.O.O.O.O.O.[Cl-].[Cl-].[Cl-].[Cr+3:10].[N:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[C:17]([O-:19])=[O:18].[NH4+]>O>[N:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[C:17]([O-:19])=[O:18].[Cr+3:10].[N:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[C:17]([O-:19])=[O:18].[N:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[C:17]([O-:19])=[O:18]

Komponenten

4

Edukt 2

HCID 166918Chromium(3+) trichloride hexahydrateHCID 69533129HCID 69533129, Verbindung

Produkt 1

HCID 151932Chromium(III) picolinateAusbeute 90 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
3 °C

Versuchsvorschrift

Aqueous chromium trichloride hexahydrate solution (23.95 g, 0.09 mol of Cr in 63 ml of water/was added dropwise over a period of 3.5 hours to an ammonium picolinate solution (271.4 g; 0.325 mol; 16.8%), pH 7.1, 73° C. in a 500 ml flask. The resulting violet solution was stirred for a further 1 hour and then slowly cooled to 3° C. After the red solid which had formed had settled out, the upper blue phase was decanted off. The solid was suspended in 100 ml of water for 30 min., and decantation was repeated. After a second suspension in 50 ml of water (30 min.), the solid was filtered off with suction and dried at 50° C. in vacuo. 33.64 g of dark red crystals was obtained (90 percent yield).

Aufarbeitung

  1. customAfter the red solid which had formed
  2. customthe upper blue phase was decanted off
  3. waitThe solid was suspended in 100 ml of water for 30 min.
  4. filtrationAfter a second suspension in 50 ml of water (30 min.), the solid was filtered off with suction
  5. customdried at 50° C. in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-3ad9b106242a4564858df2f8a96784f9
Quelldatensatz
uspto-grants-1997_12
Patentnummer
US05702930

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