Organic 2 Review Problem 322

Organic 2 Review Problem 322 - 306 PRACTICAL ORGANIC...

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306 PRACTICAL ORGANIC CHEMISTRY rise. Then boil the mixture under reflux for 2 hours, and cool it in ice-water. Now add 40 g. of powdered (or "flake") sodium hydroxide slowly to the chilled mixture, shaking the latter gently around. Avoid vigorous shaking, which may produce an emul- sion. If a solid material separates, redissolve it by the addition of a minimum of cold water. Transfer the mixture to a separating- funnel, separate the upper oily layer, and then extract the aqueous layer three times with ether (40 ml. for each extraction). Dry the united oily layer and ethereal extracts with sodium hydroxide, filter, and distil from a small Claisen distilling-flask (e.g. Fig. 4i(A) and (B), p. 65), the ethereal solution being run in slowly from a dropping-funnel as fast as the ether distils over. Then fit a capillary tube to the flask and distil the residue at water-pump pressure. 2-Ammo-4-methylthiazole distils at 124-125°/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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