9,10-DIAMINOPHENANTHRENE DIHYDROCHLORIDE synthesis

Yield:-

Reaction Conditions:

with hydrogenchloride;tin(ll) chloride in ethanol;water at 70; for 0.333333 h;Inert atmosphere;Reflux;

Steps:

32.b b) Synthesis of phenanthrene-9,1O-diamine hydrochloride

b) Synthesis of phenanthrene-9,1O-diamine hydrochloride 3.4 g (14.3 mmol) of phenanthrene-9,10-dione oxime are dissolved in refluxing ethanol (135 ml). The solution is cooled below 70 00 and 14.9 g (78.5 mmol) SnCI2 dissolved in 135 ml hydrochloric acid (32%) are added dropwise within 10 minutes. The reaction mixture starts to reflux upon the exothermic reaction. The reaction is refluxed for additional 10 minutes. After cooling to room temperature the precipitate is filtered off and is washed with ethanol. The crude product is di25 rectly used in the next reaction.

References:

WO2016/20516,2016,A1 Location in patent:Page/Page column 219