Ammonia → 2,6-Bis(tert-butylamino)-4-methylpyridin-3-yl methyl ketone

Participants

Reaction Conditions

Reaction Steps

About 60 ml. of anhydrous ammonia were condensed into a flask containing 60 ml. of methylene chloride. The reaction mixture was maintained at a temperature not in excess of -30° C. under nitrogen and a solution of 50 g. of 2-t-butyl-5-methylisoxazolium perchlorate in 100 ml. of methylene chloride was added rapidly. The reaction mixture was allowed to come to room temperature and stirred for 4 days at room temperature. The methylene chloride was then removed at reduced pressure to obtain a gummy solid which was triturated with water to obtain a yellow solid. Recrystallization of the yellow solid from methanol/water yielded the product, m.p. 128°-129° C. Its spectra were identical with those of the product of Example 4(a).

Provenance & Evidence