反应详情

温度

65 °C

53.4 g of 2,2'-dichloroazoxybenzene are stirred in 60 ml of methanol. 0.6 g of sodium hydroxide and 11.8 ml of hydrazine hydrate are added and the mixture is warmed to 65° C. After Raney nickel has been added (a total of about 0.05 g in 2-3 portions) vigorous evolution of nitrogen starts. The reduction has ended after 30 minutes. The mixture is cooled to 10° C. and diluted with water and the 2,2'-dichlorohydrazobenzene which has crystallised out is filtered off and washed with water until neutral. After the rearrangement to 3,3'-dichlorobenzidine and tetrazotisation with nitrous acid, a yield of 86% of theory is obtained.

1. temperatureThe mixture is cooled to 10° C.
2. customthe 2,2'-dichlorohydrazobenzene which has crystallised out
3. filtrationis filtered off
4. washwashed with water until neutral