Desulphurisation of 5,5-pentamethylene-4-oxazolidinone-2-thione; 5,5-pentamethyleneoxazolidine-2,4-dione
Submitted Jan 05, 2011, published Mar 05, 2011
John Davidson (email@example.com
A contribution from
A mixture of 5,5-pentamethylene-4-oxazolidinone-2-thione (0.02 mole), water (20 ml) and CCl4 was warmed up and then bromine (2 ml) added. After cooling, SO2 was passed through the mixture until the colour of bromine had disappeared. The product was extracted with ether (200 ml), the extract washed with water (30 ml) and dried over sodium sulphate. Next day the ether and CCl4 was distilled off on a water bath and the residue recrystallized from heptane (300 ml ) to afford 3.13 g (92%)
mp 112-113° Lit. mp 110-111°, 110-112°
Found: C 56.8%, H 6.6%, N 8.2% Calc. for C8H11NO3 C 56.8%, H 6.5%, N 8.25%.
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