Methyl iodide → HCID 19969448, compound

Participants

Reaction Steps

To a solution of 4-trifluoromethyl-10,11-dihydrodibenzo[b,f][1,4]thiazepin-11-one (0.295 g, 1 mmol) in DMF (20 ml) was added sodium hydride (0.1 g of 60% dispersion in oil) and the resulting mixture stirred for 30 minutes, before methyl iodide (1 equivalent) was added. After stirring for 1 hour the mixture was evaporated and the residue separated between ethyl acetate and aqueous sodium bicarbonate. The organic fractions were dried (magnesium sulphate) and evaporated. Purification of the residue by chromatography on silica, eluting with ethyl acetate/petrol (1:1, v/v), followed by recrystallisation from cyclohexane gave the title compound as colourless needles (0.121 g, m.p. 139°-141°, Rf 0.41 [silica, ethyl acetate/petrol, 1:2, v/v]).

Provenance & Evidence