306 PRACTICAL ORGANIC CHEMISTRYrise. Then boil the mixture under reflux for 2 hours, and coolit in ice-water. Now add 40 g. of powdered (or "flake") sodiumhydroxide slowly to the chilled mixture, shaking the latter gentlyaround. Avoid vigorous shaking, which may produce an emul-sion. If a solid material separates, redissolve it by the additionof a minimum ofcoldwater. Transfer the mixture to a separating-funnel, separate the upper oily layer, and then extract theaqueous layer three times with ether (40 ml. for each extraction).Dry the united oily layer and ethereal extracts with sodiumhydroxide, filter, and distil from a small Claisen distilling-flask(e.g. Fig. 4i(A) and (B), p. 65), the ethereal solution being run inslowly from a dropping-funnel as fast as the ether distils over.Then fit a capillary tube to the flask and distil the residue atwater-pump pressure. 2-Ammo-4-methylthiazole distils at124-125°/14 mm. as a colourless liquid which solidifies on cool-ing, and has m.p. 42-44°. Yield, 15-5-16 g.
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This note was uploaded on 09/19/2011 for the course CHM 2211 taught by Professor Castalleano during the Fall '06 term at University of Florida.