反応 #49390

反応方程式

water

hexamethyldisilazane

methanol

3-Iodophthalic anhydride

→

3-iodophtalimide

収率 68.0%

溶媒

DMF

反応条件

後処理

1. 1
   抽出extracted with ethyl acetate
2. 2
   洗浄The organic layer was washed with saturated brine
3. 3
   乾燥dried over anhydrous sodium sulfate
4. 4
   その他The solvent was evaporated under reduced pressure a and the residue
5. 5
   その他was purified by slurry

実験手順

3-Iodophthalic anhydride (598 mg, 2.18 mmol) was dissolved in DMF (14 mL), and the solution was added with an aqueous solution (10 mL) of hexamethyldisilazane (HMDS) (4.6 mL, 22 mmol) and methanol (0.44 mL, 11 mmol), followed by stirring at room temperature for 18.5 hours. The reaction mixture was added with water and extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure a and the residue was purified by slurry using chloroform to obtain 3-iodophtalimide (403 mg, yield 68%).

出典