Detection of Intramolecular Linkage Isomerization of a (Pseudo)tetrahedral Nickel(II) Bis(chelate)

✍ Scribed by Prof. Dr. Rudolf Knorr; Dr. Friedrich Ruf

• Book ID: 101554073
• Publisher: John Wiley and Sons
• Year: 1984
• Tongue: English
• Weight: 240 KB
• Volume: 23
• Category: Article
• ISSN: 0044-8249
• DOI: 10.1002/anie.198403681

✦ Synopsis

131 Experimenfal Procedure for 2 and 4d4b (cf. [12a]): terf-Butyllithium (15-18 mmol in pentane/hexane) is added dropwise to a solution of 1ethoxyethene (7.0 mmol) or of I-ethoxypropene (E/Z=28 :72) in 10 mL THF (or 5.0 mL pentane with 7.0 mmol TMEDA) under an inert gas atmosphere at -74"C, the mixture allowed to warm slowly to room temperature, the solvent and educt removed at 12 torr/+25"C, and the residue taken up in fresh solvent. Signals of the regenerated enol ether (for 4d4b in the same E/Z ratio) appear in the 'H-NMR spectrum only after addition of ferf-butyl alcohol.