反応 #1605822

反応方程式

5-Acetyl-8-[(4-methoxyphenyl)methoxy]-1,2-dihydroquinolin-2-one

Pyridinium tribromide

→

5-(2-bromoacetyl)-8-[(4-methoxyphenyl)methoxy]-1,2-dihydroquinolin-2-one

収率 33.1%

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   温度the reaction mixture was heated
2. 2
   温度under reflux overnight
3. 3
   ろ過The precipitate was collected by filtration
4. 4
   洗浄washed with tetrahydrofuran
5. 5
   濃縮The filtrate was concentrated under reduced pressure
6. 6
   洗浄the residue was suspension-washed with purified water (20 mL)
7. 7
   ろ過The precipitate was collected by filtration
8. 8
   洗浄washed with purified water
9. 9
   洗浄The solid was suspension-washed with ethyl acetate (20 mL)
10. 10
    ろ過collected by filtration
11. 11
    その他dried under reduced pressure

実験手順

5-Acetyl-8-[(4-methoxyphenyl)methoxy]-1,2-dihydroquinolin-2-one (1.25 g, 3.87 mmol) was dissolved in tetrahydrofuran (10 mL) and the solution was cooled to 0° C. Pyridinium tribromide (1.51 g, 4.25 mmol) was added in portions thereto and the reaction mixture was heated under reflux overnight. The precipitate was collected by filtration and washed with tetrahydrofuran. The filtrate was concentrated under reduced pressure and, thereafter, the residue was suspension-washed with purified water (20 mL). The precipitate was collected by filtration and washed with purified water. The solid was suspension-washed with ethyl acetate (20 mL), collected by filtration, and dried under reduced pressure to obtain 5-(2-bromoacetyl)-8-[(4-methoxyphenyl)methoxy]-1,2-dihydroquinolin-2-one (515 mg).

出典