تفاعل #4471

ord-76b14a9408c64659932b886070897fcf

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزThe mixture was concentrated to one half of its volume
  2. 2
    ترشيحThe mixture was filtered off
  3. 3
    غسيلwashed with water (50 ml)
  4. 4
    أخرىair-dried for 1 h
  5. 5
    تجفيفdried in vacuo over phosphorus pentoxide

الإجراء التجريبي

The product of Stage (ii) (7.28 g), potassium carbonate (9.90 g), acetone (70 ml), and dimethylsulphate (5.1 ml) were vigorously stirred at room temperature overnight under nitrogen. The mixture was concentrated to one half of its volume and then stirred with water (350 ml) for 30 min. The mixture was filtered off, washed with water (50 ml), air-dried for 1 h, and dried in vacuo over phosphorus pentoxide to give the title compound as needles (7.59 g), m.p. 157.5°-158.5°.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04725615uspto-grants-1988_02