تفاعل #2193

ord-854622046616431a8dec648c46bb4905

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةunder reflux
  2. 2
    تركيزconcentrated
  3. 3
    workup.ADDITIONWater was added to the residue
  4. 4
    استخلاصthe mixture was extracted with ethyl acetate
  5. 5
    غسيلThe ethyl acetate layer was washed with water
  6. 6
    تجفيفdried over anhydrous magnesium sulfate
  7. 7
    تركيزconcentrated
  8. 8
    أخرىThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=10:1)

الإجراء التجريبي

4-chloro-4'-mercaptomethylbenzophenone (16.0 g), ethyl bromide (7.4 g) and potassium hydroxide (4.3 g) were added to methanol (250 ml), and the mixture was stirred for 30 minutes under reflux. The reaction mixture was cooled to room temperature and then concentrated. Water was added to the residue, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with water and then dried over anhydrous magnesium sulfate and concentrated. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=10:1) to obtain the desired product 14.0 g, melting point: 33° to 34° C., yield: 79%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05728699uspto-grants-1998_03