Homoallyl bromide → HCID 13298149, compound

Participants

Reaction Conditions

Reaction Steps

47 g (0.25 mol) of the monosodium salt of 3-methylxanthine (prepared as described in Example 1b) and 34.8 g (0.25 mol) of 97% strength 1-bromo-3-butene in 750 ml of dimethylformamide are stirred for 8 hours at 110° C. Thereafter, the precipitated sodium bromide is removed by filtration of the still hot reaction mixture, the filtrate is concentrated in vacuo, the solid residue is dissolved in 250 ml of 2N sodium hydroxide solution, the solution is heated to about 65° C. and 2N hydrochloric acid is added, while stirring, until the pH reaches 9. After cooling, the solid formed is filtered off under suction, washed salt-free with water, rinsed with methanol and then dried in vacuo.

Provenance & Evidence