Hexathio-digermanates and -distannates: A New Type of Dimeric Tetrahedral Ion

✍ Scribed by Priv.-Doz. Dr. Bernt Krebs; Siegfried Pohl; Willy Schiwy

• Publisher: John Wiley and Sons
• Year: 1970
• Tongue: English
• Weight: 237 KB
• Volume: 9
• Category: Article
• ISSN: 0044-8249
• DOI: 10.1002/anie.197008972

✦ Synopsis

AIBNIsl). The mixture is then cooled rapidly, filtered through a G4 frit, and freed from solvent and organic impurities a t 2OoC in a high vacuum. Sublimation of the residue in a high vacuum then gives analytically pure ( 3 )

[330 mg, 97 % based on (I)].

A solution of AIBN (117 mg, 0.71 mmole) and CO(CgH5)2 (327 mg, 1.73 mmoles) in benzene (20 ml) is heated for 15 h under reflux (> 99 % decomposition of the AIBN [61).

The excess of C O ( C ~H S ) ~

is extracted with aqueous NH4Cl solution, and the benzene phase is dried over CaC12.

Further working up as above affords ( 3 ) (297 mg, 81 % based o n AIBN).