تفاعل #1241687

ord-5f370e4411bf4a4c8a5872d49fc21b43

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe oxidation inhibitor, bis(dithiobenzil) nickel is prepared
  2. 2
    workup.ADDITIONby adding
  3. 3
    أخرىequipped
  4. 4
    أخرىis formed
  5. 5
    درجة الحرارةThe reaction mixture is cooled

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04490265uspto-grants-1984_12