Ketone dineopentyl-, preparation

Ketone dineopentyl-, preparation of, 54, 97 Ketone, heptyl phenyl, 53, 78 Ketones, alkylation of, 54, 48 Clemmensen reduction of, 53,... 

Under stirring, a-bromo(dineopentyl) ketone (33.6 g, 0.135 mol), cooled by an ice-water bath, was triturated over a period of 30min with a solution of t-BuOK in /-BuOH (120 mL, l.OM, 0.12mol) (prepared by addition of potassium metal to freshly distilled, sodium-dried t-BuOH and standardized by back titration of an aliquot with 0.1 N aq HCl). When the mixture solidified, the iee-bath was removed. The mixture was concentrated at ca. 60 °C (25 Torr) and trap-to-trap distilled at 25 -100 "C (0.1 Torr). Recrystallization of the distillate from pentane at — 78 "C gave /ranr-2,3-di-/er/-butylcyclopropanone yield 16.8 g (75%) bp 75-77°C/20Torr mp 24-26 C the yield can vary from 30 to 75%. 

An ethereal soln. of dineopentyl ketone added during 2 hrs. to 2,4,6-trimethyl-phenylmagnesium bromide prepared from bromomesitylene and Mg in ether, refluxed 2 hrs., then acetic anhydride in ether added during 2 hrs. with icecooling, and stirring continued 1 hr. - 2,2,6,6-tetramethylhept-3-en-4-yl acetate. Y 90%. F. e. s. H. G. Hauthal, P. Kluge, and H. Schmidt, J. pr. 29, 296 (1965). 

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See also in sourсe #XX -- [ , ]

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