Methyl preparation

A solution of 192 g of 1 -phenethyl-4-hydroxy-4-aminomethyl piperidine in BOO cc of diethyi-carbonate is heated for 1 /i hours to refiux at about B0°C in the presence of sodium methylate (prepared for immediate use from 2 g of sodium). After this time, the ethyl alcohol formed during the reaction is slowly distilled while the maximum temperature is reached. The excess ethyl carbonate is distilled under reduced pressure. A crystallized residue Is then obtained, which is stirred with 400 cc of water and 400 cc of ether. The solution is filtered and 125 g (77.6%) of practically pure product melting at 232°C to 233°C, are obtained. 

C,Hk, 1,3-Cyclopentadiene, 1-methyl-, preparation and purification of, 27 52 titanium complex, 27 52 vanadium complex, 27 54, 55 QH,Oj, Ascorbic acid, platinum complex, 27 283... 

L. Mond and his co-workers discovered it in 1888. The platinum methyls, prepared in 1907 by W. J. Pope, were amongst the first-known transition metal alkyls, and the discovery by W. Reppe in 1940 that Ni complexes catalyse the cyclic oligomerization of acetylenes produced a surge of interest which was reinforced by the discovery in I960 of the jr-allylic complexes of which those of Pd arc by far the most numerous. 

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