反応 #6011

反応方程式

acetyl chloride

aluminum chloride

dimethylformamide

benzoselenazolinone

→

6-Acetylbenzoselenazolinone

反応条件

後処理

1. 1
   温度After cooling
2. 2
   workup.STIRRINGthe mixture is homogenized
3. 3
   温度It is heated to 70°-80° C. on an oil bath
4. 4
   workup.STIRRINGwith stirring
5. 5
   温度heating
6. 6
   温度is maintained at a temperature of 80°-90° C. for a time T of approximately 4 h 30 min
7. 7
   その他on crushed ice
8. 8
   その他dried
9. 9
   洗浄washed with boiling cyclohexane
10. 10
    その他recrystallized in toluene

実験手順

12 grams (0.09 mol) of aluminum chloride are introduced into a ground-necked flask. 3.1 cm3 (0.04 mol) of dimethylformamide are added dropwise with stirring. After cooling, two grams (0.01 mol) of benzoselenazolinone are added and the mixture is homogenized. It is heated to 70°-80° C. on an oil bath with stirring, and 0.01 to 0.012 mol of acetyl chloride is then added. heating is maintained at a temperature of 80°-90° C. for a time T of approximately 4 h 30 min. The mixture is hydrolyzed on crushed ice. The product is drained, dried, and washed with boiling cyclohexane and recrystallized in toluene.

出典