bromine; sodium hydrogencarbonate; chloroform; water;
reactants are commercially availlable.
institut de recherches chimiques et biologiques appliquees (i.r.c.e.b.a.), us5322846, a1, (1994) step 1: synthesis of 2-amino-5-bromo-4-methylthiazole a solution of bromine in chloroform, consisting of 66.7 ml (1.30 mol) of br2 in 1000 ml of chcl3, is added dropwise to a solution of 120 g (1.05 m ol) of 2-amino-4-methylthiazole in 2300 ml of chcl3, with stirring. a precipitate appears during the addition. stirring is maintained for 48 h. the reaction medium is then filtered and the hydrobromid e is washed with methylene chloride and then with pentane. the hydrobromide is dissolved in 2000 ml of water and then rendered basic by the addition of 850 ml of a 10percent aqueous solution of sodium bicarbonate. this solution is then extracted with methylene chloride. the organic phase is dried over sodium sulfate. a crystalline residue is obtained after removal of the solvent under vacuum. brow n crystals: m=155 g (crude yield: 76percent) m.p.kb =112°-113°c . 1 h nmr (delta ppm, dmso) 2.05 (s, 3h, ch3); 7.15 (s, 2h, nh2).
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