Synthesis, Structure, and Physical Properties of the Organic–Inorganic Hybrid Salt (BEDT-TTF)6[PMo12O40]·(4CH3CN·6H2O)
✍ Scribed by Mohamedally Kurmoo; Mario Bonamico; Carlo Bellitto; Vincenzo Fares; Fulvio Federici; Philippe Guionneau; Laurent Ducasse; Hiroshi Kitagawa; Peter Day
- Publisher
- John Wiley and Sons
- Year
- 1998
- Tongue
- English
- Weight
- 266 KB
- Volume
- 10
- Category
- Article
- ISSN
- 0935-9648
No coin nor oath required. For personal study only.
✦ Synopsis
Bromohexyl)-3¢,4¢-ethylenedioxy)-2,2¢-bithiophene (3): Into a roundbottomed flask were introduced EDOT (5.9 g, 41.4 mmol) and 150 mL of tetrahydrofuran (THF). The mixture was cooled to ±40 C and butyllithium, 2.5 M in hexanes (19 mL, 47.5 mmol), was added rapidly. After 1 h stirring, tributyltin chloride (10.11 ml, 37.3 mmol) was added and the mixture was stirred for 30 min. The solution was stirred overnight at room temperature, washed with water, and extracted with Et 2 O. After removal of the solvent and distillation of the unreacted EDOT the crude product was used directly for the next step.
Compounds 4b (2.6 g, 6.03 mmol) and 6b (1 g, 3.1 mmol), Pd(PPh 3 ) 4 (35 mg, 0.03 mmol), and 35 mL of toluene were heated at 85 C under nitrogen for 20 h. After addition of 1 N aqueous HCl the solution was extracted with Et 2 O. Solvent removal left an oil, which was purified by column chromatography (silica gel, ethylacetate/petroleum ether 1:20), giving 600 mg (50 %) of a yellow oil. 1 H NMR (CDCl 3 ) 7. 25 (d, 1H, 3