تفاعل #2446139

ord-b7f8cd85edd84aa3979183814cebc8ab

المذيبات

ظروف التفاعل

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

المعالجة

  1. 1
    استخلاصthe solution was extracted with ethyl acetate (3×150 ml)
  2. 2
    غسيلThe organic phase was washed with water (2×200 mL)
  3. 3
    تجفيفdried over MgSO4
  4. 4
    أخرىevaporated
  5. 5
    أخرىaffording a yellow solid, which

الإجراء التجريبي

To a solution of 1,2,5,6-tetrahydro-pyrrolo[3,2,1-ij]quinolin-4-one (10.0 g, 55.8 mmol) in 100 ml dry DMF was added dropwise a solution of N-bromosuccinimide (10.4 g, 58.6 mmol) in 150 ml dry DMF at 0° C. The mixture was stirred at 0° C. for 2 h, then 400 ml water was added and the solution was extracted with ethyl acetate (3×150 ml). The organic phase was washed with water (2×200 mL), then dried over MgSO4 and evaporated, affording a yellow solid, which was purified by crystallization from acetone/ether providing pure 8-bromo-1,2,5,6-tetrahydro-pyrrolo[3,2,1-ij]-quinolin-4-one (12.8 g, 50.8 mmol, 91%) as pale yellow needles.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08685960B2uspto-grants-2014_04