Bromo-methane solution

Preparation of the title compound by interaction of dimethyl sulfoxide and bromo-methane, sealed into a resin-coated glass bottle and heated at 65°C, led to an explosion after 120 h. The isolated salt thermally decomposes above 180°C to produce formaldehyde and a residue of methanesulfonic acid. In solution in dimethyl sulfoxide, the salt begins to decompose after several hours at 74—80°C (after exposure to light), the exothermic reaction accelerating with vigorous evolution of vapour (including formaldehyde and dimethyl sulfide), the residue of methanesulfonic acid finally attaining 132°C. Some white solid, probably poly-formaldehyde, is also produced. The explosion... 

A V-bis [2-(dimethylamino)ethyl] -N1 ft-dimethyl-1,2-ethanediamine] bromo-palladium(II) bromide is a yellow diamagnetic solid. It melts at 210° with decomposition. It is very hygroscopic and must be handled and stored in a moisture-free atmosphere. It is soluble in water, chloroform, and dichloro-methane but insoluble in most other common laboratory solvents. The H nmr spectrum in D20 exhibits a single resonance at 2.60 ppm for the methyl protons. The electronic spectrum obtained on an aqueous solution is characterized by an absorption maximum at 352 nm (e = 792 L mole-1 cm"1). 

In Schlenk tube, l-bromo-2-iodobenzene (2.5 g, 8.8 mmol), diphenylphosphine (1.4 niL, 8.0 mmol), triethylamine (1.5 mL, 11 mmol), and a catalytic amount of Pd(PPh3)4 (50 mg, 4.4 x 10 mmol) were dissolved in 2 mL of toluene under nitrogen atmosphere. The solution was heated at 80 °C under stirring for 16 h. The reaction mixture was washed with brine and extracted with diethyl ether three times. The organic layer was dried over anhydrous magnesium sulfate, and concentrated to dryness. Column chromatography on silica gel (hexane/dichloro-methane = 4 1) afforded the titled compound as a white solid [33]. 

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