Intramolecular Electron Transfer from Iron(II) to Cobalt(III) through 2,4,6-Pyridinetricarboxylate as Mediating Bridging Ligand
✍ Scribed by Dipl.-Chem. Horst Bertram; Prof. Dr. Karl Wieghardt
- Publisher
- John Wiley and Sons
- Year
- 1978
- Tongue
- English
- Weight
- 195 KB
- Volume
- 17
- Category
- Article
- ISSN
- 0044-8249
No coin nor oath required. For personal study only.
✦ Synopsis
Compound ( 1 ) (0.68g, 4mmol) is dissolved under N2 in anhydrous tetrahydrofuran (50 ml). To this solution, cooled to -113"C, is added dropwise a solution of tert-butyllithium in n-pentane (3ml,5.1 mmol; ca. 1.7 M solution). After 15min the olefin or carbonyl compound (8mmol) is addedC6]. The solution is rapidly warmed to room temperature and stirred for a further 3 h"]. After workup with water/chloroform, the dried (Na2S04) CHCl3 extract is evaporated down in a waterpump vacuum and the crude product is fractionated in a bulb tube [(4a)], recrystallized from ethyl acetate/light petroleum [(4b)], or chromatographed over silica gel. Eluent: ethyl acetate [(3 d), (4 e)], benzene/acetone 7: 3 [(3 c)], ethyl acetate/light petroleum (low) 12:4 [(4a)], 10:2 [(3e)], ethyl acetate/methanol/light petroleum 7: 1 : 14 [(3 u), (3 b)].