تفاعل #80723

معادلة التفاعل

AlCl3

N-3,3-dimethylacryloyl-3-bromoaniline

Compound 17

N-3,3-dimethylacryloyl-3-bromoaniline

→

title compound

4,4-Dimethyl-2-oxo-1,2,3,4-tetrahydro-7-bromoquinoline

المذيبات

CH2Cl2

ظروف التفاعل

المعالجة

1. 1
   أخرىInto a 500 ml round-buttom flask was placed
2. 2
   أخرىkept at 0° C
3. 3
   أخرىslowly quenched with small chunks of ice-cubes and finally with water
4. 4
   غسيلThe aqueous layer was washed with CH2Cl2
5. 5
   تجفيفthe organic layer was dried over Na2SO4
6. 6
   أخرىThe solvent was evaporated
7. 7
   أخرىthe residue purified by recrystallization from EtOAc-hexane

الإجراء التجريبي

Into a 500 ml round-buttom flask was placed 13.52 g (101 mmol) of AlCl3 under nitrogen purge and kept at 0° C. Thereafter, 22.41 g of N-3,3-dimethylacryloyl-3-bromoaniline (Compound 17) in 350 ml CH2Cl2 was slowly added by syringe. The reaction mixture was stirred at 0° C. for 72 h, and thereafter slowly quenched with small chunks of ice-cubes and finally with water. The aqueous layer was washed with CH2Cl2 and the organic layer was dried over Na2SO4. The solvent was evaporated and the residue purified by recrystallization from EtOAc-hexane to give the title compound as off-white solids.

المصدر