反応 #80723

反応方程式

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

溶媒

CH2Cl2

反応条件

後処理

1. 1
   その他Into a 500 ml round-buttom flask was placed
2. 2
   その他kept at 0° C
3. 3
   その他slowly quenched with small chunks of ice-cubes and finally with water
4. 4
   洗浄The aqueous layer was washed with CH2Cl2
5. 5
   乾燥the organic layer was dried over Na2SO4
6. 6
   その他The solvent was evaporated
7. 7
   その他the residue purified by recrystallization from EtOAc-hexane

実験手順

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.

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