反应详情

An aqueous solution of 1800 g of hydroxylammonium sulfate solution (25% strength) is made up (=5.39 mol of hydroxylamine). 79.0 g of moist hydrogenation catalyst are added thereto. The free sulfuric acid in the solution is partly neutralized by means of 36.7 g of 50% strength sodium hydroxide solution (=0.458 mol) over a period of 2 minutes. While stirring, the mixture is thermostated to 50° C. and 477.9 g (4.87 mol) of cyclohexanone are introduced over a period of 30 minutes by means of a Desaga pump. The reactor is flushed and the hydrogenation is commenced with vigorous stirring. The hydrogen is introduced via the sparging tube during the entire time. After 100% of theory of H2 have been reached, 167 g (2.88 mol) of acetone are fed in at 50° C. Hydrogenation is subsequently continued. Finally, CIPHAS is confirmed as main product. The free hydroxylamine derivative can be obtained by reaction with sodium hydroxide. A work-up is not carried out.

1. customis thermostated to 50° C.
2. customThe reactor is flushed
3. additionThe hydrogen is introduced via the sparging tube during the entire time
4. customare fed in at 50° C