反应详情

Hydrogen chloride was passed into a mixture of 60 g (1 mole) of glacial acetic acid and 111.0 g (1 mole) of pivaloyl cyanide at 20° to 25° C. and under 8 bars for 5 hours. The reaction mixture was then let down and poured onto an excess of a saturated sodium bicarbonate solution. The mixture was extracted three times with 200 ml of methylene chloride each time. The combined organic phases were washed with 200 ml of water, dried over sodium sulphate and concentrated by distilling off the solvent in vacuo. The residue which remained crystallized after a short time. Recrystallization from petroleum ether gave 97 g (75.2% of theory) of trimethylpyruvic acid amide of melting point 68° to 69° C.

1. extractionThe mixture was extracted three times with 200 ml of methylene chloride each time
2. washThe combined organic phases were washed with 200 ml of water
3. dry with materialdried over sodium sulphate
4. concentrationconcentrated
5. distillationby distilling off the solvent in vacuo
6. customThe residue which remained crystallized after a short time
7. customRecrystallization from petroleum ether