Sulfuric Acid → HCID 178441961, compound

Participants

Reaction Steps

111 grams (1 mole) of pivaloyl cyanide were dissolved in 200 ml of glacial acetic acid and treated at 0° to +5° C. with 152 grams (1.5 moles) of 97% sulfuric acid. Within 2 hours there were led in 112.2 grams (2 moles) of isobutylene at 0° to +5° C. In connection with the one hour post reaction at 20° C. there were added at the same temperature 200 ml of glacial acetic acid and 108 grams of water. The mixture was heated at boiling in a very slow current of nitrogen for 4 hours, whereby 92 grams (82% of that employed) of isobutylene escaped and was caught in a cooling trap. The mixture was treated at 80° C. with 100 grams of water and subsequently with 92.4 grams (0.87 mole) of thiocarbohydrazide. It was stirred for a further 10 minutes at 95° to 100° C. and then cooled. By filtration there were isolated 162 grams of the triazinone (I) having a melting point of 208°-210° C. (81% of theory).

Provenance & Evidence