Hexane 1,6-diiodo

Hexane 1.6-Diiodo-dodecalluoro-EI0b,. 483/490 (Educt) ElOb,. 79/610 (E duct) ElOb,. 5 (Educt)... 

Catalytic amounts of [Pd(PPh3)4] (chiffres ) and Cul were added to a solution of dithienophosphole 80 (1.73 g, 1.5 mmol) and l,4-diiodo-2,5-bis(octyloxy)benzene (0.88 g, 1.5 mmol) in N-methylpyrrolidinone (80 mL). The light-yellow reaction mixture was then stirred for 48 h at 200 °C, after which time the color changed to orange-red. The solution was then cooled to room temperature, the solvent evaporated under vacuum and the resulting amorphous solid taken up in a small amount of THF (ca. 5 mL). The suspension was filtered, precipitated into hexane and the residue dried under vacuum to yield 80 as a reddish brown pow-... 

Octakis[f-butyl]-l,2,3,4,5-telluratetrastannolane1 All operations are performed under an argon atmosphere with oxygen-free solvents. Hydrogen telluride is passed for 1 h through a solution of 5.0 g (4.2 mmol) of 1,4-diiodo-l, 1,2,2,3,3,4,4-octakis[f-butyl]tetrastannane n a mixture of 100 ml of toluene and 1 ml of triethylamine. The mixture is then filtered to remove precipitated triethylammonium iodide, the solvent is evaporated from the filtrate, and the residue is recrystallized from chloroform/hexane yield 2.4 g (55%) m.p. 170° (dec.). 

Diiodo tris(3,5-dimethylpyrazolyl)hydroborato molybdenum(III) is an air-stable, black, crystalline solid that dissolves in chloroform, dichloromethane, and toluene, but is only slightly soluble in hexane. It reacts with alcohols (see below), and is best stored for prolonged periods under dry nitrogen. The infrared spectrum (KBr disc) shows vNO 1700 cm-1 and vBH 2555 cm-1, and the 220 MHz H nmr spectrum in CDC13 shows signals attributable to the pyrazolyl protons at = 6.09 (area 1) and 5.86 (area 2), the phenyl protons at = 7.13, 7.27 (area 5), and the pyrazolyl methyl protons at = 2.77 (area 3), 2.58 (area 3), 2.29 (area 6), and 2.19 (area 6). 

Procedure for preparation of 2,6-diazasemibullvalene 5-lf (Type II, Method A) from cyclic 2y-disubstituted 1,4-diiodo-l,3-dienes 5-7b /-BuLi (4.0 mmol, 1.6 M in pentane) was added to a solution of cyclic 2,3-disubstituted l,4-diiodo-l,3-diene 5-7b (1.0 mmol) in diethyl ether (10 mL) in a 20-ml Schlenk tube at —78 °C (diy ice/ acetone). The reaction mixture was then stirred at —78 °C for 30 min to generate 1,4-dilithio-1,3-diene, and then, the reaction mixmre was stirred at room temperature for 30 min. After addition of /-BuCN (2.4 mmol, 264 pi) at -78 °C, the mixmre was heated to reflux and maintained for 3 h. Then, r-BuOCl (1.0 mmol, 119 pi) was added and the reaction mixture was kept at room temperature for 2 h. After dried up, the reaction mixture was extracted with hexane (20 mL) and filtered. The solvent was evaporated in vacuum. Repeat this extraction-filtration-drying procedure for three times to afibrd 2,6-diazasemibullvalene 5-lf. 

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