تفاعل #54745

ord-ea6bdc68b4f04cdbad0f3478d9dc9e09

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحthe solid product is filtered off with suction
  2. 2
    غسيلAfter washing with water
  3. 3
    استخلاصextracted once with water
  4. 4
    تجفيفThe organic phase is then dried over sodium sulphate
  5. 5
    ترشيحfiltered
  6. 6
    تركيزconcentrated in a vacuum evaporator
  7. 7
    ترشيحfiltered off with suction
  8. 8
    أخرىdried
  9. 9
    أخرىThere is obtained a yield of 3.3 g of substance

الإجراء التجريبي

6.1 g (0.02 mole) of the 3-(4-chlorophenyl)-5-bromo-5-methyl-oxazolidine-2,4-dione, produced in a manner analogous to that described in Example 1, and 33.2 g (0.2 mole) of potassium iodide are placed, together with a spatula tip of benzyltriethylammonium chloride, in 50 ml of water, and the mixture is stirred at 50° for 7 days. It is then cooled to room temperature, and the solid product is filtered off with suction. After washing with water, the crude product is taken up in methylene chloride, and extracted once with water. The organic phase is then dried over sodium sulphate, filtered, and concentrated in a vacuum evaporator. The substance remaining behind is digested with a small amount of ether/petroleum ether, then filtered off with suction and dried. There is obtained a yield of 3.3 g of substance having a melting point of 132°-142°.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04150144uspto-grants-1979_04