تفاعل #2446140

معادلة التفاعل

acetone ether

1,2,6,7-tetrahydro-5H-pyrido[3,2,1-ij]quinolin-3-one

N-bromosuccinimide

water

→

9-Bromo-1,2,6,7-tetrahydro-5H-pyrido[3,2,1-ij]quinolin-3-one

المذيبات

DMF

DMF

ظروف التفاعل

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 1,2,6,7-tetrahydro-5H-pyrido[3,2,1-ij]quinolin-3-one (9.1 g, 48.6 mmol) in 100 ml dry DMF was added dropwise a solution of N-bromosuccinimide (9.08 g, 51.0 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 9-bromo-1,2,6,7-tetrahydro-5H-pyrido[3,2,1-ij]quinolin-3-one (6.53, 24.5 mmol, 50%) as pale yellow needles.

المصدر