반응 #2383145
ord-a9cac86babbc43bc992f891a06a78792
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후처리
- 1기타The oxidation inhibitor, bis(dithiobenzil) nickel is prepared
- 2workup.ADDITIONby adding
- 3기타equipped
- 4기타is formed
- 5온도The reaction mixture is cooled
실험 절차
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.