Reaktion #7364

Reaktionsgleichung

NaOH

ZrCl4

2,2,6,6-tetramethyl-3,5-heptanedione

water

→

tetrakis(2,2,6,6-tetramethyl-3,5-heptanedionato)zirconium

Ausbeute 98.2%

Lösungsmittel

methanol

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeTo the resulting solution, a solution, which had been obtained
2. 2
   workup.ADDITIONwas added over a period of about 5 minutes
3. 3
   workup.STIRRINGwith stirring
4. 4
   workup.STIRRINGThen, stirring
5. 5
   workup.WAITwas performed for 1 hour
6. 6
   SonstigeThe resulting crystals were collected by centrifugation
7. 7
   Sonstigedried

Vorschrift

To 177 g of methanol, 43.7 g (0.216 mol) of 2,2,6,6-tetramethyl-3,5-heptanedione of 91% purity was dropwise added with stirring. To the resulting solution, a solution, which had been obtained by dissolving 12.7 g (0.054 mol) of ZrCl4 of 99% purity in 218 g of methanol and cooled to room temperature, was added over a period of about 5 minutes. The reaction was conducted for 1 hour with stirring, and 590 g of water was added over a period of 50 minutes. Then, stirring was performed for 1 hour. The resulting solution was adjusted to pH 6.6 with a 20% NaOH solution. The resulting crystals were collected by centrifugation and then dried. Thus, 43.9 g (yield: 98.2%) of tetrakis(2,2,6,6-tetramethyl-3,5-heptanedionato)zirconium was obtained.

Quelle