تفاعل #1605822

ord-973ea9e53b9a48198face942c0e6fa1a

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe reaction mixture was heated
  2. 2
    درجة الحرارةunder reflux overnight
  3. 3
    ترشيحThe precipitate was collected by filtration
  4. 4
    غسيلwashed with tetrahydrofuran
  5. 5
    تركيزThe filtrate was concentrated under reduced pressure
  6. 6
    غسيلthe residue was suspension-washed with purified water (20 mL)
  7. 7
    ترشيحThe precipitate was collected by filtration
  8. 8
    غسيلwashed with purified water
  9. 9
    غسيلThe solid was suspension-washed with ethyl acetate (20 mL)
  10. 10
    ترشيحcollected by filtration
  11. 11
    أخرىdried under reduced pressure

الإجراء التجريبي

5-Acetyl-8-[(4-methoxyphenyl)methoxy]-1,2-dihydroquinolin-2-one (1.25 g, 3.87 mmol) was dissolved in tetrahydrofuran (10 mL) and the solution was cooled to 0° C. Pyridinium tribromide (1.51 g, 4.25 mmol) was added in portions thereto and the reaction mixture was heated under reflux overnight. The precipitate was collected by filtration and washed with tetrahydrofuran. The filtrate was concentrated under reduced pressure and, thereafter, the residue was suspension-washed with purified water (20 mL). The precipitate was collected by filtration and washed with purified water. The solid was suspension-washed with ethyl acetate (20 mL), collected by filtration, and dried under reduced pressure to obtain 5-(2-bromoacetyl)-8-[(4-methoxyphenyl)methoxy]-1,2-dihydroquinolin-2-one (515 mg).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09072734B2uspto-grants-2015_07