Reaktion #1241687

Reaktionsgleichung

btah

benzoin

phosphorus sulfide

nickel chloride

dithiobenzoin

hydrogen sulfide

→

bis(dithiobenzil) nickel

Lösungsmittel

dioxane

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe oxidation inhibitor, bis(dithiobenzil) nickel is prepared
2. 2
   workup.ADDITIONby adding
3. 3
   Sonstigeequipped
4. 4
   Sonstigeis formed
5. 5
   TemperaturThe reaction mixture is cooled

Vorschrift

The oxidation inhibitor, bis(dithiobenzil) nickel is prepared by adding a mixture of 100 grams of benzoin, 150 grams of phosphorus sulfide and 700 ml of dioxane to a 5 liter, single necked flask equipped with heating mantle and water cooled condenser. The above-described mixture is, then, refluxed for 2 hours, during which the thiophosphoric ester of dithiobenzoin is formed and hydrogen sulfide is evolved. The reaction mixture is cooled and a solution of 50 grams of nickel chloride (hydrated) in 200 ml of water is added to the flask and heated (212° F.) for 2 hours on a steam btah. Black crystals of bis(dithiobenzil) nickel are formed and collected by filtering the cooled solution. Purification is effected by extraction with boiling toluene.

Quelle