Water → 6-Bromo-3,4-dihydroquinolin-2(1H)-one
反応式
[NH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][C:2]1=[O:11].[Br:12]N1C(=O)CCC1=O.O.CCOCC>CN(C=O)C>[Br:12][C:7]1[CH:6]=[C:5]2[C:10](=[CH:9][CH:8]=1)[NH:1][C:2](=[O:11])[CH2:3][CH2:4]2参加物
6
反応条件
- 温度
- 0 °C
実験手順
To a solution of 3,4-dihydro-1H-quinolin-2-one (10.0 g, 67.9 mmol) in 100 ml dry DMF was added dropwise a solution of N-bromosuccinimide (12.7 g, 71.3 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 washing with cold ether providing pure 6-bromo-3,4-dihydro-1H-quinolin-2-one (13.6 g, 60.3 mmol, 89%) as colorless needles.
後処理
- extractionthe solution was extracted with ethyl acetate (3×150 ml)
- washThe organic phase was washed with water (2×200 ml)
- dry with materialdried over MgSO4
- customevaporated
- customaffording a yellow solid which
- customwas purified
出典と根拠
- ORDレコード
- ord-2c76de3fb4934d3d8f7361fe1776060d
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08541404B2
反応ノート
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