反応 #347079

反応方程式

4-nitro-1-naphthylamine

HCl

HCl

HCl

sodium nitrite

→

expected product

1-Hydrazino-4-nitronaphthalene Hydrochloride

溶媒

AcOH

water

反応条件

後処理

1. 1
   workup.WAITThe mixture is left
2. 2
   その他to rise to RT
3. 3
   workup.STIRRINGthe reaction mixture is kept stirring for 2 hours 30 minutes
4. 4
   ろ過It is filtered
5. 5
   ろ過the mixture is filtered again

実験手順

A solution of 1.9 g of sodium nitrite in 10 ml of water is added to a suspension, cooled to -5° C., of 5.2 g of 4-nitro-1-naphthylamine in 150 ml of concentrated HCl, 100 ml of 1N HCl and 150 ml of AcOH. The mixture is left stirring for 1 hour 15 minutes at a temperature of between -5° C. and 0° C. It is cooled to -15° C., and a solution of 12.5 g of stannous chloride dihydrate in 30 ml of concentrated HCl is added very slowly. The temperature is allowed to rise to RT and the reaction mixture is kept stirring for 2 hours 30 minutes. It is filtered, the solid is then taken up with water and the mixture is filtered again. 5.9 g of the expected product are obtained.

出典