反応 #2383145

反応方程式

benzoin

phosphorus sulfide

nickel chloride

dithiobenzoin

hydrogen sulfide

→

bis(dithiobenzil) nickel

溶媒

dioxane

water

water

反応条件

後処理

1. 1
   その他The oxidation inhibitor, bis(dithiobenzil) nickel is prepared
2. 2
   workup.ADDITIONby adding
3. 3
   その他equipped
4. 4
   その他is formed
5. 5
   温度The reaction mixture is cooled

実験手順

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 bath. Black crystals of bis(dithiobenzil) nickel are formed and collected by filtering the cooled solution. Purification is effected by extraction with boiling toluene.

出典