反応 #1726708

反応方程式

water

2-bromoacetophenone

potassium phthalimide

→

2-phthalimido-acetophenone

収率 86.0%

溶媒

DMF

反応条件

後処理

1. 1
   抽出extracted with chloroform (300 ml
2. 2
   洗浄The combined organic phases were washed with sodium hydroxide (200 ml, 0.2 N), water (2×100 ml) and brine (100 ml)
3. 3
   乾燥dried over magnesium sulfate
4. 4
   濃縮concentrated in vacuo
5. 5
   ろ過recovered by filtration
6. 6
   洗浄washed with ether (100 ml)
7. 7
   その他dried in vacuo

実験手順

A solution of 2-bromoacetophenone (30.0 g, 151 mmol) in DMF (120 ml) was treated with potassium phthalimide (30.8 g, 166 mmol) portionwise at ambient temperature, and then heated to 40° C. for 3.5 hr. The cooled mixture was poured into water (600 ml) and extracted with chloroform (300 ml then 100 ml). The combined organic phases were washed with sodium hydroxide (200 ml, 0.2 N), water (2×100 ml) and brine (100 ml), dried over magnesium sulfate and concentrated in vacuo. The resulting cream solid was suspended in ether (100 ml), recovered by filtration, washed with ether (100 ml) and dried in vacuo to yield pure 2-phthalimido-acetophenone as a white solid (34.3 g, 86%).

出典